专利号:US-11040938-B2 优先权日:2016-07-27 标 题 :Continuous flow process for the synthesis of phenylhydrazine salts and substituted phenylhydrazine salts 发明人:MA BING; PAN SHUAI 权利人:SHANGHAI HYBRID—CHEM TECH; SHANGHAI HYBRID CHEM TECH 摘要:The present invention provided a continuous flow process for the synthesis of phenylhydrazine salts and substituted phenylhydrazine salts. Diazotization, reduction, acidic hydrolysis and salifying with acids are innovatively integrated together. Using acidic liquids of aniline or substituted aniline, diazotization reagents, reductants and acids as raw materials, phenylhydrazine derivative salts is obtained through the synthesis process, which is a three-step continuous tandem reaction including diazotization, reduction, acidic hydrolysis and salifying. The described synthesis process is a kind of integrated solutions, which is carried out in an integrated reactor. The feed inlets of the integrated reactor are continuously filled with raw materials. In the integrated reactor, diazotization, reduction, acidic hydrolysis and salifying are carried out continuously and orderly, and phenylhydrazine salts or substituted phenylhydrazine salts is obtained in the outlet of the integrated reactor without interruption. The total reaction time is no more than 20 min.
专利号:WO-2025108921-A1 优先权日:2023-11-22 标 题 :Synthesis of radiopharmaceutical agents 发明人:AUZELOUX PHILIPPE; LEVESQUE SOPHIE; GALMIER MARIE-JOSÈPHE; CHEZAL JEAN-MICHEL 权利人:INST NAT SANTE RECH MED; UNIV CLERMONT AUVERGNE; CENTRE LUTTE CONTRE LE CANCER 摘要:Synthesis of radiopharmaceutical agents It is disclosed a method to synthesize a compound of formula (I), or a pharmaceutically acceptable salt thereof: Formula (I), (I) said process comprising contacting a trialkylstannane precursor of formula (II), or a pharmaceutically acceptable salt thereof: Formula (II), (II) with an alkali metal salt of a radionuclide selected from the group consisting of 123I, 124I, 125I, 131I, 211At, in appropriate acidic conditions and in presence of a peroxide ROOH in an 10 appropriate concentration. Said method is particularly suited for synthesizing [131I]N-(2- diethylaminoethyl)-6-iodoquinoxaline-2-carboxamide, providing a notable reduction in the quantity of side products, allowing a much purer finished product, while making use of reagents which are adapted to the constraints which need to be met when developing a product for clinical use and, more in particular, to the constraints to be met in order to 15 adapt the process for being fully automated.
专利号:US-12221452-B2 优先权日:2017-10-04 标题:Synthesis of cantharidin 发明人:DAVIDSON MATTHEW GENE; EKLOV BRIAN MATTHEW; WUTS PETER; LOERTSCHER BRAD MELVIN; SCHOW STEVEN R 权利人:VERRICA PHARMACEUTICALS INC 摘要:The invention provides synthetic methods for the preparation of cantharidin and analogs thereof. In one aspect, the invention provides an improved Diels-Alder cycloaddition to generate a key intermediate en route to cantharidin and analogs thereof. In certain embodiments, the new Diels-Alder reaction involves reacting Compound (2) in the presence of furan, and in the absence of acid or increased pressure, in an aprotic polar solvent with slight warming, to yield Compound (1) in favorable yield and exo-endo ratio. In another aspect, the invention also provides a new Diels-Alder reaction between compounds of Formula (III) and furan to yield compounds of Formula (IV), which can then be transformed into cantharidin or analogs thereof. In yet another aspect, the invention describes a new palladium-mediated carbonylation providing another key intermediate en route to cantharidin and analogs thereof. In addition to synthetic methods, present invention also provides compounds (i.e., intermediates) useful in the synthesis of cantharidin and analogs thereof. Compounds provided herein may have biological activity, and therefore may be used in the treatment of diseases or conditions (e.g., infectious diseases and skin conditions).
专利号:US-11485804-B2 优先权日:2017-10-17 标题:Method for the synthesis of fluoropolymers 发明人:D'APRILE FIORENZA; KAPELYUSHKO VALERIY; KENT BRADLEY LANE; BRINATI GIULIO; PONTA LAURA 权利人:SOLVAY SPECIALTY POLYMERS IT 摘要:The present invention relates to a fluorosurfactant-free emulsion polymerization method for the synthesis of a fluoropolymer, more in particular of a VDF-based polymer.
专利号:US-9394394-B2 优先权日:2013-09-30 标题:Synthesis of chlorotrifluoroethylene-based block copolymers by iodine transfer polymerization 发明人:THENAPPAN ALAGAPPAN; AMEDURI BRUNO; LOPEZ GERALD 权利人:HONEYWELL INT INC 摘要:Methods for the synthesis of CTFE-based block copolymers through iodine transfer polymerization are disclosed. In an exemplary embodiment, a method includes reacting a fluoromonomer “Mâ€? with a chain transfer agent of the formula X—Y or Y—X—Y, wherein X represents a C 1 -C 3 hydrocarbon, a C 1 -C 6 hydrofluorocarbon, C 1 -C 6 hydrochlorofluorocarbon, or C 1 -C 6 fluorocarbon and Y represents iodine or bromine, in the presence of a radical initiator, to form a macro-initiator of the formula: X-poly(M)-Y or Y-poly(M)-X-poly(M)-Y, wherein poly(M) represents a polymer of the fluoromonomer. The method further includes reacting the macro-initiator with chlorotrifluoroethylene (CTFE) in the presence of a radical initiator to form a diblock or a triblock CTFE-based block copolymer of the formula: X-poly(M)-block-poly(CTFE) or PCTFE-block-poly(M)-X-poly(M)-block-PCTFE.
专利号:US-11008285-B2 优先权日:2017-03-27 标 题 :Process for synthesis of mesotrione 发明人:GHARDA KEKI HORMUSJI; MATHUR SUCHET SARAN; JAIN NANDKUMAR JANARDAN; SATHE SHEKHAR VISHWANATH; DAMANIA PRAGNESH DALPATRAM 权利人:GHARDA CHEMICALS LTD 摘要:The present disclosure relates to a process for synthesis of mesotrione. The process comprises reacting 4-toluene sulfonyl chloride with alkali metal sulphite and alkali metal bicarbonate to obtain alkali metal toluene-4-sulfinate. The alkali metal toluene-4-sulfinate is reacted with alkali metal salt of monochloroacetic acid to obtain 4-methylsulfonyl toluene. Further, 4-methylsulfonyl toluene is nitrated to obtain 2-nitro-4-methylsulfonyl toluene. 2-nitro-4-methylsulfonyl toluene is oxidized and then halogenated to obtain 2-nitro-4-methylsulfonylbenzoyl halide. 2-nitro-4-methylsulfonylbenzoyl halide is reacted with alkali metal salt of 1,3-cyclohexanedione to obtain 3-(2-Nitro-4-methylsulfonylbenzoyloxy)cyclohexen-1-one which is reacted with base, a third fluid medium and cyanide ion source to obtain an amorphous mesotrione. The present disclosure also discloses the steps of converting the amorphous mesotrione to crystalline mesotrione having purity greater than 99%. The process of the present disclosure for preparing mesotrione is rapid, economic, and environment friendly.