Water → 4-Acetyl-1-benzylpyrrolidin-2-one

HRID 1198608노트

반응식

HRID 1198608 반응식
[CH2:1]([N:8]1[CH2:12][CH:11]([C:13](=[O:18])[CH2:14]C([O-])=O)[CH2:10][C:9]1=[O:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[Na+].O>CS(C)=O>[C:13]([CH:11]1[CH2:12][N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:9](=[O:19])[CH2:10]1)(=[O:18])[CH3:14]

참가 물질

5

반응물 3

HCID 962WaterHCID 5234Sodium ChlorideHCID 19102755HCID 19102755, 화합물

생성물 1

HCID 100820724-Acetyl-1-benzylpyrrolidin-2-one수율 83.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 3-(1-benzyl-2-oxopyrrolidin-4-yl)-3-oxopropanoate (24.0 g, 0.083 mole) and sodium chloride (10.6 g, 0.181 mole) in dimethylsulfoxide (105 mL)/water (4.4 mL) was heated at 135° with stirring for 16 hours. On cooling the reaction mixture was poured onto ice water (900 mL) and extracted with dichloromethane (800 mL). The organic phase was washed with water (4×500 mL) and dried (MgSO4). The solvent was removed under reduced pressure to give 4-acetyl-1-benzyl-2-pyrrolidinone (15.0 g, 83%) as a brown oil.

후처리

  1. temperaturewas heated at 135°
  2. temperatureOn cooling the reaction mixture
  3. additionwas poured onto ice water (900 mL)
  4. extractionextracted with dichloromethane (800 mL)
  5. washThe organic phase was washed with water (4×500 mL)
  6. dry with materialdried (MgSO4)
  7. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-fb770d900b0e4b18ad802b5fc0f1a253
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05281612

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