Acetic Anhydride → 1-Benzyl-3-acetamidopyrrolidine

HRID 1382754ノート

反応式

HRID 1382754 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 41983391-Benzyl-3-acetamidopyrrolidine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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-1benzylpyrrolidine (9.0 g) as oil.

後処理

  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

出典と根拠

ORDレコード
ord-0737739d98af477188f59651a1809b48
出典データセット
uspto-grants-1989_02
特許番号
US04808584

反応ノート

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