Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Detailed Action
A request for continued examination under 37 CFR 1.114, including the fee set forth in 37 CFR 1.17(e), was filed in this application after final rejection. Since this application is eligible for continued examination under 37 CFR 1.114, and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114. Applicant's submission filed on 3/20/26 has been entered.
Claims 1-19 and 21-22 are pending in this application. Claims 16-19 remain withdrawn from consideration being drawn to the non-elected invention.
As a result, claims 1-15 and 21-22 are being examined in this Office Action.
Claim Rejections – 35 USC 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102 of this title, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
The factual inquiries set forth in Graham v. John Deere Co., 383 U.S. 1, 148
USPQ 459 (1966), that are applied for establishing a background for determining obviousness under 35 U.S.C. 1 03(a) are summarized as follows:
1. Applicant Claims
2. Determining the scope and contents of the prior art.
3. Ascertaining the differences between the prior art and the claims at issue, and resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claim 1-15 and 21-22 are rejected under AIA 35 U.S.C. 103(a) as being obvious over Liu et al. (CN 1557697, published 2004, see English Translation used herein), in view of Peng et al. (CN 105668628, published 2016, see English Translation used herein), further in view of Stieger et al. (Crystallization-Science and Technology, 2012, Ch 7: Recrystallization of Active Pharmaceutical Ingredients, page 183).
Determination of the Scope and Content of the Prior Art
(MPEP §2141.01)
Liu et al. teaches the production of crystalline ammonium tetrathiomolybdate by contacting the molybdenum compound, ammonium heptamolybdate tetrahydrate (ammonium paramolybdate), with water and ammonia in a reaction vessel under stirring and heat (40 to 60 degrees C) to obtain a molybdenum compound solution. Then adding ammonium sulfide to the molybdenum compound solution in an amount corresponding to a S:Mo molar ratio in a range of 4-6:1, the solution was kept at a temperature of room temperature to 90 degrees C for 0.5 to 3 hours. The reaction was cooled to room temperature and then the resultant slurry was crystallized for 8 to 24 hours. The mixture was then fIltered, washed with water, then with absolute ethanol, then dried to produce highly pure crystals of ammonium tetrathiomolybdate in high yield. (entire page 8, claims, examples)
Liu et al. teaches “adding distilled water in an amount of 3-6 times by volume” to the reaction solution and controlling the reactant concentrations, since after reaction, the vessel was cooled and used to crystallize the ammonium tetrathiomolybdate product. (page 8-9, examples 1 and 2)
Liu et al. exemplifies isolating the ammonium tetrathiomolybdate product as a dark red needle-shaped crystal with an XRD spectrum, elemental analysis, TG-DTA with a match to the standard and to the theoretical values. Liu et al. also teaches “In addition, as shown in Figure 2, the ammonium tetrathiomolybdate prepared using the method of the present invention is decomposed into MoS3 (theoretical weight loss 26.1%, measured weight loss 26.5%) at 130-200ºC and is further decomposed into MoS2 (theoretical weight loss 12.3%, measured weight loss 12.7%) at 260-370ºC in nitrogen atmosphere. The aforementioned results indicate that the obtained sample is ammonium tetrathiomolybdate, and the sample has relatively high purity.” (page 9, first paragraph, last sentence to page 10, first paragraph)
Liu et al.’s results give an approximate estimate of 97% purity, which would align with Liu et al.’s “relatively high purity” description. This is calculated from the difference in the theoretical weight loss versus the measured weight loss from the MoS3 and MoS2 decompositions. Thus it would be reasonable to interpret an approximate 97% purity as the “relatively high purity” for the ammonium tetrathiomolybdate product, which is based on applicant’s experiments from the measured weight loss of the MoS3 and MoS2 decompositions.
Furthermore, since Liu et al. teaches after the reaction, the solution was cooled to room temperature and then the resultant slurry was crystallized for 8 to 24 hours, this reads on applicant’s limitation for maintaining the slurry at a temperature in a range of 10 to 30 degree C for at least 2 hours.
Ascertainment of the Difference Between Scope the Prior Art and the Claims
(MPEP §2141.012)
Liu et al. is deficient in the sense that it does not teach applicant’s purity, particular reaction time of at least 5 hours and adding the ethanol crystallization solvent to the product slurry.
Peng et al. teaches the industrial mass production of highly pure crystalline ammonium tetrathiomolybdate (ATTM). Peng et al. teaches contacting the molybdenum compound, ammonium heptamolybdate, in a reaction vessel under stirring with an aqueous ammonium sulfide corresponding to a S:Mo molar ratio in a range of 4-8:1, maintaining the reaction mixture at a temperature in a range of room temperature to 1000C for a reaction time of 0.5 to 5 hours, cooling to room temperature and crystallizing for 0.5 to 24 hours; and filtering and washing with water, then ethanol and drying to obtain crystalline ATTM. (paragraphs 14-22, 26; examples; claims)
Peng et al. teaches the solvents used in the purification process for washing the crystals can be water, methanol, ethanol, ethylene glycol, petroleum ether, n-hexane, tetrahydrofuran and toluene. (paragraph 22)
Thus Peng et al. teaches the use of ethanol in the purification process for washing the crystals.
Peng et al. teaches the elemental analysis of their ammonium tetrathiomolybdate product they obtain is consistent with the theoretical values and thus of “very high” purity (paragraphs 32, 38, 44, 51, 57, 63).
Thus it would be reasonable to expect Peng et al.’s “very high” purity to be equal or greater than Liu et al.’s approximate 97% purity or “relatively high purity”, based on Peng et al.’s elemental analysis of their ammonium tetrathiomolybdate product.
Stieger et al. teaches that the use of antisolvents can be used to create supersaturation of the solution for crystallization. Stieger et al. teaches a common solvent-antisolvent pair is water and ethanol. Also Stieger et al. teaches that antisolvent crystallization is similar to cooling crystallization. The composition of the crystallization medium can affect both the crystal form and crystal habit of the product. (page 193, first and second paragraphs and table, first entry row)
Finding of Prima Facie Obviousness Rationale and Motivation
(MPEP §2142-2143)
Therefore, it would be prima facie obvious to one of ordinary skill in the art at the time of the invention, to utilize Stieger et al.’s ethanol as an antisolvent for Liu et al.’s crystallization of ammonium tetrathiomolybdate, with a reasonable expectation of success, especially since Peng et al. already uses ethanol in their purification process for washing the crystals.
Thus it would be obvious to try to utilize ethanol as the antisolvent in the ammonium tetrathiomolybdate water solution during the crystallization step, since Stieger et al. teaches ethanol is a common antisolvent pair to water and to create supersaturation of the solution for crystallization. Furthermore, Stieger et al. teaches the equivalency of antisolvent and cooling crystallization. Note that an express suggestion to substitute one equivalent component or process for another is not necessary to render such substitution obvious. In re Fout, 675 F.2d 297, 213 USPQ 532 (CCPA 1982).
With regard to Applicant’s limitation for adding ethanol, at about 35 volume %, as the crystallization solvent, it is the position of the examiner that one of ordinary skill in the art, at the time of the invention, would through routine and normal experimentation optimize the amount of ethanol in the purification process, in order to increase the yield of product and lower the impurities, especially since both Liu et al. and Peng et al. teach the use of ethanol in the purification process, during the washing step. Because, both Liu et al. and Peng et al. teach adding ethanol at the washing step in the purification process, it would be obvious to add ethanol earlier in the purification process, as an antisolvent in the crystallization process.
Furthermore, it would be prima facie obvious to one of ordinary skill in the art at the time of the invention, to obtain an approximate 97% purity for the ammonium tetrathiomolybdate product, which would meet applicant’s limitation for “less than 9 % (w/w) of [MoOS3]2- impurity”, since the maximum amount of any impurity would be approximately 3%, based on Liu et al.’s and Peng et al.’s analysis of their ammonium tetrathiomolybdate product. It would also be obvious to optimize the purity of the ammonium tetrathiomolybdate product since pure forms of known compounds are obvious.
When claiming a purer form of a known compound, it must be demonstrated that the purified material possess properties and utilities not possessed by the unpurified material. Ex parte Reed, 135 U.S.P.Q. 34, 36 (P.O.B.A. 1961), on reconsideration, Ex parte Reed, 135 U.S.P.Q. 105 (P.O.B.A. 1961).
It has been well established that the mere purity of compound, in itself, does not render a substance unobvious Ex Parte Gray (BPAI 1989) 10 PQ2D 1922.
As stated in Aventis Pharma Deutschland Gmbh and King Pharmaceuticals, Inc., v. Lupin, Ltd., 84 USPQ2d 1197:
“The ‘reason or motivation' need not be an explicit teaching that the claimed compound will have a particular utility; it is sufficient to show that the claimed and prior art compounds possess a ‘sufficiently close relationship . . . to create an expectation,' in light of the totality of the prior art, that the new compound will have ‘similar properties' to the old.”
“However, if it is known that some desirable property of a mixture derives in whole or in part from a particular one of its components, or if the prior art would provide a person of ordinary skill in the art with reason to believe that this is so, the purified compound is prima facie obvious over the mixture even without an explicit teaching that the ingredient should be concentrated or purified….”
“Ordinarily, one expects a concentrated or purified ingredient to retain the same properties it exhibited in a mixture, and for those properties to be amplified when the ingredient is concentrated or purified; isolation of interesting compounds is a mainstay of the chemist' s art. If it is known how to perform such an isolation, doing so ‘is likely the product not of innovation but of ordinary skill and common sense.'”
Furthermore, it would be obvious to optimize Liu et al.’s reaction time by lengthening it to Peng et al.’s 5 hours reaction time, in order to optimize the purity and yield of the ammonium tetrathiomolybdate product.
Thus with regard to applicant's limitation regarding reaction/addition times, solvents amounts and product purities, it is the position of the examiner that one of ordinary skill in the art, at the time of the invention, would through routine and normal experimentation determine the optimization of these limitations to provide the best effective variable depending on the result desired. Because the art teaches varying reaction and crystallization times, as well as the use and amount of different solvents in the purification process, and well as obtaining high purity product, the examiner asserts that the reaction/addition times, solvents amounts and product purities are art recognized result-effective variables. Thus it would be obvious in the optimization process to optimize the reaction/addition times, solvents amounts and product purities. The applicant does not show any unusual and/or unexpected results for the limitations stated. Note that the prior art provides the same effect desired by the applicant, the formation of highly pure ammonium tetrathiomolybdate product.
Response to Arguments
Applicant’s arguments have been considered but are not persuasive for the following reasons:
The examiner acknowledges applicant’s argument for unexpected benefits regarding the antisolvent feature, temperature control and sulfide quench strategy tied to yield.
The examiner is unable to assess if applicant’s arguments reflect true unexpected results since applicant has not provided reaction conditions and comparative yields.
The USPTO relies on the applicants to provide evidence of a nexus between rebuttal evidence and the claimed invention. As the Court of Appeals for the Federal Circuit (CAFC) stated in In re Huang, 100 F.3d 135, 139-140 (Fed. Cir. 1996). This hard evidence would include tables or data and not mere argument. Also see Amicus Inc. v. Post-Tension of Texas Inc., 5 USPQ2d 1735 (1987); Ecolochem v. Mobile Water Technology, 8 USPQ2d 1065 (1988); Lantech Inc. v. Kaufman Co. of Ohio Inc., 12 USPQ2d, 1076 (1989).
The examiner acknowledges applicant’s argument that there is no motivation to include ethanol as an antisolvent to the processes of Liu and Peng.
The examiner does not agree with applicant’s argument since the examiner has included Stieger et al. is the 103 rejection above. Stieger et al. teaches that the use of antisolvents can be used to create supersaturation of the solution for crystallization. Stieger et al. teaches a common solvent-antisolvent pair is water and ethanol. Also Stieger et al. teaches that antisolvent crystallization is similar to cooling crystallization.
Therefore, it would be prima facie obvious to one of ordinary skill in the art at the time of the invention, to utilize Stieger et al.’s ethanol as an antisolvent for Liu et al.’s crystallization of ammonium tetrathiomolybdate, with a reasonable expectation of success, especially since Peng et al. already uses ethanol in their purification process for washing the crystals.
Thus it would be obvious to try to utilize ethanol as the antisolvent in the ammonium tetrathiomolybdate water solution during the crystallization step, since Stieger et al. teaches ethanol is a common antisolvent pair to water and to create supersaturation of the solution for crystallization. Furthermore, Stieger et al. teaches the equivalency of antisolvent and cooling crystallization. Note that an express suggestion to substitute one equivalent component or process for another is not necessary to render such substitution obvious. In re Fout, 675 F.2d 297, 213 USPQ 532 (CCPA 1982).
Applicant also argues that adding an additional solvent, such as ethanol, would introduce impurities and thus be avoided. This argument makes little sense since ethanol can be purchased at extremely high purities, and because the introduction of the common ethanol antisolvent is used to purify the dissolved product, not to add additional impurities. Both the use of two solvents (solvent-antisolvent pair) for crystallization and the use of ethanol as the antisolvent for aqueous crystallization solutions are old in the art.
Conclusion
No claim is allowed.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to Jennifer Cho Sawyer whose telephone number is (571) 270 1690. The examiner can normally be reached on Monday-Friday 9 AM - 6 PM PST.
If attempts to reach the examiner by telephone are unsuccessful, the examiner's supervisor, Renee Claytor can be reached on (571) 272-8394. The fax phone number for the organization where this application or proceeding is assigned is 571-274-1690.
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Jennifer Cho Sawyer
Patent Examiner
Art Unit: 1691
/RENEE CLAYTOR/Supervisory Patent Examiner, Art Unit 1691