Water → (3S,4S)-1-Benzyl-4-(tert-butoxycarbonylamino-methyl)-pyrrolidine-3-carboxylic Acid

HRID 2193553노트

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C(OC(N1CC[C@@H](NC2C=CC(N3C[C@H](CNC(=O)C)OC3=O)=CC=2F)C1)=O)(C)(C)C.C([O:34][C:35]([C@H:37]1[C@@H:41]([CH2:42][NH:43][C:44]([O:46][C:47]([CH3:50])([CH3:49])[CH3:48])=[O:45])[CH2:40][N:39]([CH2:51][C:52]2[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=2)[CH2:38]1)=[O:36])C.O.[OH-].[Li+].O>C1COCC1>[CH2:51]([N:39]1[CH2:40][C@H:41]([CH2:42][NH:43][C:44]([O:46][C:47]([CH3:48])([CH3:49])[CH3:50])=[O:45])[C@H:37]([C:35]([OH:36])=[O:34])[CH2:38]1)[C:52]1[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=1

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온도: 40 °C

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To a solution of 2.9 (3R, 4R) and (3S, 4S)-1-benzyl-4-(tert-butoxycarbonylamino-methyl)-pyrrolidine-3-carboxylic acid ethyl ester (8.0 mmol) in 50 ml THF were added 671 mg lithium hydroxide mono hydrate (, 16 mmol) and 0.5 ml water. The solution was stirred at 40° C. and the reaction monitored by TLC. After 72 h the solvent was evaporated, the residue dissolved in dichloromethane, washed with water and brine, dried over Mg sulfate, filtered and evaporated. The residue was crystallized from a dichloromethane/hexane mixture.

후처리

customAfter 72 h the solvent was evaporated
dissolutionthe residue dissolved in dichloromethane
washwashed with water and brine
dry with materialdried over Mg sulfate
filtrationfiltered
customevaporated
customThe residue was crystallized from a dichloromethane/hexane mixture

출처 및 근거

ORD 기록: ord-f406e256d96646acb6282da856e4a168
출처 데이터셋: uspto-grants-2012_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08329908B2

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