CAS: 477600-74-1; N-Methyl-N-((3R,4R)-4-Methylpiperidin-3-yl)-7H-Pyrrolo[2,3-D]Pyrimidin-4-Amine

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CAS号24211-54-9 (S)-5-羟基哌啶-2酮 | CAS号1500-85-2 4-氨基-7H-吡咯[2,3-d]嘧啶 | CAS号176966-77-1 tert-butyl (5S)... | CAS号176966-79-3 (4R,5S)-tert-bu...

2,4-二氯-7H吡咯[2,3-D]嘧啶置于三乙基硅烷,5%-Palladium/activated Carbon,Potassium Carbonate,溶剂黄146体系中,用 甲醇,水 作为反应溶剂,化学反应 10.17H,反应生成 N-甲基-N-((3R,4R)-4-甲基哌啶-3-基)-7H-吡咯并[2,3-D]嘧啶-4-胺
参考文献:一种枸橼酸托法替尼的制备方法
标题:一种枸橼酸托法替尼的制备方法
摘要:本发明公开了一种枸橼酸托法替尼的制备方法.它是将有机溶剂,化合物3,5%湿钯碳和乙酸搅拌至悬浮,从通道a进入微反应器,同时烷基硅烷从通道b进入微反应器,在微反应器控温20~30oc进行反应,经后处理得到化合物2;将醇类溶剂,化合物2,氰乙酸乙酯和dbu搅拌均匀后从通道a进入微反应器,将柠檬酸溶于水和醇类溶剂的混合溶剂中,从通道b进入微反应器,在微反应器内控温70~80oc进行反应,降温析晶,得到枸橼酸托法替尼.该方法反应条件可控,操作简单,避免了使用易燃易爆的氢气带来危险,安全性更高,并可实现瞬间反应完成,大大的缩短反应时间,并且脱苄反应和酰化反应彻底,后处理简单,适合规模化工业大生产.

专利信息

专利号:US-8309716-B2
优先权日:2005-07-29
标题 :Pyrrolo[2,3-d]pyrimidine derivatives: their intermediates and synthesis
发明人：RUGGERI SALLY GUT; HAWKINS JOEL M; MAKOWSKI TERESA M; RUTHERFORD JENNIFER L; URBAN FRANK J
权利人:RUGGERI SALLY GUT; HAWKINS JOEL M; MAKOWSKI TERESA M; RUTHERFORD JENNIFER L; URBAN FRANK J; PFIZER
摘要:This invention relates to methods and intermediates useful for the synthesis of pyrrolo[2,3-d]pyrimidine compounds. Specifically novel synthetic methods and intermediates for the synthesis of 3-{(3R,4R)-4-methyl-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-amino}-piperidin-1-yl)-3-oxo-propionitrile and its corresponding citrate salt are disclosed.

专利号:US-11827598-B1
优先权日:2022-07-15
标 题:Preparation method of tofacitinib citrate
发明人：HSU YAO-LUNG; HSIEH KUANG-CHAN; CHENG HUI-WEN; Yang zong-han
权利人:CHUNGHWA CHEMICAL SYNTHESIS & BIOTECH CO LTD
摘要:The present disclosure provides a preparation method of tofacitinib citrate, which comprises the following steps: passing an intermediate TOF-2 into hydrogen at a normal pressure in the presence of a catalyst to obtain an intermediate TOF-3; in the presence of a solvent and a base, under a reduced pressure of −490 mmHg to −760 mmHg, and at a temperature of 10° C. to 25° C., reacting TOF-3 with ethyl cyanoacetate to generate an intermediate TOF-4; heating and dissolving TOF-4 and citric acid in a solvent, and performing separation by cooling to obtain tofacitinib citrate. The present disclosure obtains tofacitinib citrate with high yield, high purity and low impurities by changing a gas flow rate and a reaction temperature and pressure of a hydrogenation reaction. Therefore, the preparation method is suitable for industrial production.

专利号:US-9828380-B2
优先权日:2015-04-10
标题 :Efficient method for the preparation of tofacitinib citrate
发明人：BONANOMI JACOPO; DEFIORE STELLA; NOVO BARBARA
权利人:OLON SPA
摘要:Disclosed is a novel process for the synthesis of tofacitinib citrate on an industrial scale with high yields and purity starting with cis-(1-benzyl-4-methyl-piperidin-3-yl)methylamine bis-hydrochloride racemate (intermediate VIII), which comprises:n 1. Condensation between intermediates VII and VIII to give intermediate VI 2. Hydrogenation of intermediate VI to give intermediate V 3. Resolution of intermediate V to give intermediate IV with enantiomeric purity >99% 4. Release of intermediate IV in a basic medium to give intermediate III 5. N-acylation reaction of intermediate III to give II (tofacitinib) 6. Salification of intermediate II to give tofacitinib monocitrate (I)

专利号:CN-105693728-A
优先权日:2014-11-29
标 题:Synthesis method of JAK inhibitor tofacitinib

专利号:PT-1913000-E
优先权日:2005-07-29
标题 :DERIVATIVES OF PYRROLE [2,3-D] PYRIMIDINE, ITS INTERMEDIATE SUBSTANCES AND SYNTHESIS PROCESS