Trifluoroacetic acid → 3-Amino-1-benzhydryl-pyrrolidin-2-one

HRID 1786557

반응식

HRID 1786557 반응식
C(OC(=O)[NH:7][CH:8]1[CH2:12][CH2:11][N:10]([CH:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:9]1=[O:26])(C)(C)C.C(C(O)=O)(F)(F)F>C(Cl)Cl>[NH2:7][CH:8]1[CH2:12][CH2:11][N:10]([CH:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:9]1=[O:26]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 57597570(1-Benzhydryl-2-oxo-pyrrollidin-3-yl)-carbamic acid tert-butyl ester

생성물 1

HCID 575975623-Amino-1-benzhydryl-pyrrolidin-2-one수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To the solution of (1-benzhydryl-2-oxo-pyrrollidin-3-yl)-carbamic acid tert-butyl ester (41) (1.2 g, 3.26 mmol) in CH2Cl2 (20 ml) was added CF3CO2H (8 ml). The resulting mixture was stirred under nitrogen at room temperature overnight. The reaction was then concentrated under reduced pressure. The residue was dissolved in ethyl acetate and washed with saturated sodium hydrogen carbonate (20 ml). The organic was dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using CH2Cl2: MeOH (10:1) to give the desired product in 97% yield.

후처리

  1. concentrationThe reaction was then concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with saturated sodium hydrogen carbonate (20 ml)
  4. dry with materialThe organic was dried over MgSO4
  5. customevaporated to dryness
  6. customThe resulting residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-13e9753f36934bee8bf2fae8a1e16e7b
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07507760B2

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