Trifluoroacetic acid → (1R,3S,5R)-2-Aza-bicyclo[3.1.0]hexane-3-carboxylic acid (2-fluoro-3-trifluoro methoxy-phenyl)-amide trifluoroacetate

HRID 1527599노트

반응식

HRID 1527599 반응식
C(OC([N:8]1[C@H:13]([C:14](=[O:28])[NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22][C:23]([F:26])([F:25])[F:24])[C:17]=2[F:27])[CH2:12][C@@H:11]2[C@H:9]1[CH2:10]2)=O)(C)(C)C.[C:29]([OH:35])([C:31]([F:34])([F:33])[F:32])=[O:30]>C(Cl)Cl>[F:32][C:31]([F:34])([F:33])[C:29]([OH:35])=[O:30].[F:27][C:17]1[C:18]([O:22][C:23]([F:26])([F:24])[F:25])=[CH:19][CH:20]=[CH:21][C:16]=1[NH:15][C:14]([C@@H:13]1[CH2:12][C@@H:11]2[C@@H:9]([CH2:10]2)[NH:8]1)=[O:28]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68283686(1R,3S,5R)-3-(2-Fluoro-3-trifluoromethoxy-phenylcarbamoyl)-2-aza-bicyclo[3.1.0]hexane-2-carboxylic acid tert-butyl ester

생성물 1

HCID 86673879(1R,3S,5R)-2-Aza-bicyclo[3.1.0]hexane-3-carboxylic acid (2-fluoro-3-trifluoro methoxy-phenyl)-amide trifluoroacetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of ((1R,3S,5R)-3-(2-fluoro-3-trifluoromethoxy-phenylcarbamoyl)-2-aza-bicyclo[3.1.0]hexane-2-carboxylic acid tert-butyl ester (2.56 g, 6.33 mmol) in CH2Cl2 (20 mL) was added TFA (10 mL, 130 mmol) and the solution was stirred at RT for 16 h. CH2Cl2 was concentrated, the residue was suspended in MeOH, concentrated again and dried under high vacuum to give the desired material which was used without further purification in the next step. MS: 305 [M+H]+; tR (HPLC conditions c): 3.55 min.

후처리

  1. concentrationCH2Cl2 was concentrated
  2. concentrationconcentrated again
  3. customdried under high vacuum

출처 및 근거

ORD 기록
ord-c0db9e3e4a684c44b693303b39c736a0
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085555B2

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