Acetic Anhydride → 1-Benzyl-3-acetamidopyrrolidine

HRID 1722084노트

반응식

HRID 1722084 반응식
[NH2:1][CH:2]1[CH2:6][CH2:5][N:4]([CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:3]1.[C:14](OC(=O)C)(=[O:16])[CH3:15].[OH-].[Na+]>C(Cl)Cl>[C:14]([NH:1][CH:2]1[CH2:6][CH2:5][N:4]([CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:3]1)(=[O:16])[CH3:15]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 27566131-Benzyl-3-aminopyrrolidine

생성물 1

HCID 41983391-Benzyl-3-acetamidopyrrolidine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Amino-1-benzylpyrrolidine [8.3 g, prepared by a method of G. C. Helsley et al., J. Med. Chem. 11, 1034 (1968)] was dissolved in methylene chloride (40 ml) and thereto acetic anhydride (5.3 g) was added dropwise with stirring under cooling with ice-water and the mixture was stirred for 1.5 hours. After addition of 2N sodium hydroxide (40 ml), the mixture was extracted with methylene chloride. The extract was washed with water and dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure to give 3-acetylamino-1-benzylpyrrolidine (9.0 g) as oil.

후처리

  1. stirringthe mixture was stirred for 1.5 hours
  2. extractionthe mixture was extracted with methylene chloride
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationby distilling off the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-f066582dc1404881bae77d9826dce7f1
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853469

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