专利号:US-9029421-B2 优先权日:2008-06-02 标 题 :Process for the synthesis of arformoterol 发明人:HALDAVANEKAR VAISHALI VAMAN; PRABHU MANGESH; RAO DHARMARAJ RAMACHANDRA; KANKAN RAJENDRA NARAYANRAO 权利人:HALDAVANEKAR VAISHALI VAMAN; PRABHU MANGESH; RAO DHARMARAJ RAMACHANDRA; KANKAN RAJENDRA NARAYANRAO; CIPLA LTD 摘要:The present invention provides a process for preparing a compound of formula (VI) or a salt thereof, the process comprising: (i) reacting 4-methoxyphenyl acetone with an amine of formula (VIII) under conditions of reductive amination to produce a compound of formula (II) or a salt thereof, wherein there is no isolation of an imine intermediate formed during the reductive amination; (ii) condensing the compound (II) or the acid addition salt thereof with an α-haloketone of formula (III) to produce the compound of formula (IV); (iii) reducing the compound (IV) to a compound of formula (V); and (iv) reducing the compound (V) to the compound of formula (VI), wherein the reduction is carried out in the presence of either (1) a hydrogen donating compound in the presence of a hydrogen transfer catalyst; or (2) ammonium formate using a hydrogenation catalyst, wherein R 1 and R 2 are independently optionally substituted arylalkyl, and Hal is selected from chloro or bromo.
专利号:US-8962839-B2 优先权日:2010-11-19 标题:Chiral spiro-pyridylamidophosphine ligand compound, synthesis method therefor and application thereof 发明人:ZHOU QILIN; XIE JIANHUA; LIU XIAOYAN; XIE JIANBO; WANG LIXIN 权利人:ZHOU QILIN; XIE JIANHUA; LIU XIAOYAN; XIE JIANBO; WANG LIXIN; ZHEJIANG JIUZHOU PHARMA SCIENCE & TECHNOLOGY CO LTD 摘要:The present invention relates to a chiral spiro-pyridylamidophosphine ligand compound, synthesis method therefor and application thereof. The chiral spiro-pyridylamidophosphine compound is a compound having a structure of Formula (I), a racemate or optical isomer thereof, or a catalytically acceptable salt thereof, and is mainly characterized by having a chiral spiro-dihydro-indene skeleton in its structure. The chiral spiro-pyridylamidophosphine compound may be synthesized with optical active 7-diaryl/alkylphosphino-7′-amino-1,1′-spiro-dihydro-indene or substituted 7-diaryl/alkylphosphino-7′-amino-1,1′-spiro-dihydro-indene having a spiro-skeleton as chiral starting material. The chiral spiro-pyridylamidophosphine compound may be used as a chiral ligand in asymmetric hydrogenation of a carbonyl compound catalyzed by iridium, in which the reaction activity is very high, the amount of the catalyst may be 0.0001 mol %, and the enantioselectivity of the reaction is up to 99.9% ee.
专利号:US-5502183-A 优先权日:1992-01-28 标 题 :Steroid intermediates and processes for their preparation 发明人:ANDREWS DAVID R; SUDHAKAR ANANTHA R 权利人:SCHERING CORP 摘要:PCT No. PCT/US93/00211 Sec. 371 Date Jul. 25, 1994 Sec. 102(e) Date Jul. 25, 1994 PCT Filed Jan. 26, 1993 PCT Pub. No. WO93/15103 PCT Pub. Date Aug. 5, 1993.Novel steroids having a 9 alpha -hydroxy or a 9 alpha -carbonate substituent can be prepared from 9 alpha -hydroxyandrostenedione and can be utilized in the synthesis of commercially valuable corticosteroids such as betamethasone. The 9 alpha -carbonates are prepared by reaction of the corresponding 9 alpha -hydroxy steroid with a sequence of excess base, trialkylsilyl chloride, alkyl haloformate and alkanol or by using excess base, alkyl haloformate and alkoxide. 9 alpha -Carbonate-17-keto compounds can be treated with lithium acetylide and a lithium salt to afford the corresponding 17 alpha -ethynyl-17 beta -hydroxy-9 alpha -carbonate. This compound is then esterified with a novel series of reagents to give the 17-ester which can be reduced the corresponding 17-allene. Oxidation of this allene to the bis-epoxide compound, followed by treatment with an alkali metal salt of a carboxylic acid under phase transfer conditions gives the 17 alpha -hydroxy 21-ester 9 alpha -carbonate. Elimination of the 9 alpha -carbonate group affords the a 17 alpha -hydroxy, 9(11)ene, which in a few subsequent steps can be converted to a variety of commercially important corticosteroids. Novel 9 alpha -carbonate compounds are prepared in the various reaction steps.
专利号:CA-2724882-A1 优先权日:2008-06-02 标 题:Process for the synthesis of arformoterol
专利号:US-9441053-B2 优先权日:2013-07-11 标 题 :Analytical method for detecting sulfated oligosaccharides 发明人:WANG CHUNGYAO; HUANG IMIN; WU CHIAYEN; CHIANG YUNGTE; CHAO HELEN 权利人:SCINOPHARM TAIWAN LTD 摘要:The present invention describes an analytical method for detecting and quantitating poly-sulfated oligosaccharides, including Fondaparinux sodium, using hydrophilic interaction ultra-performance liquid chromatography (HILIC-UPLC) coupled with a charged aerosol detector (CAD) or a mass spectrometer (MS). This analytical method provides in-process control in a total synthesis of highly sulfated oligosaccharides by separation, quantification and mass identification. Systems and conditions utilizing such methods are also provided.
专利号:US-2015210629-A1 优先权日:2008-06-02 标题 :Process for the Synthesis of Arformoterol
参考文献:10.1007/s00216-006-0535-x 摘要:Larsen EH, Lobinski R, Burger-Meÿer K, Hansen M, Ruzik R, Mazurowska L, Rasmussen PH, Sloth JJ, Scholten O, Kik C. Uptake and speciation of selenium in garlic cultivated in soil amended with symbiotic fungi (mycorrhiza) and selenate. Analytical and Bioanalytical Chemistry. 2006 Jun 13;385(6):1098. doi: 10.1007/s00216-006-0535-x.