Methanol → HCID 577835, 화합물

HRID 1885621노트

반응식

HRID 1885621 반응식
[C:1]1([CH3:16])[CH:6]=[CH:5][C:4]([N:7]2[C:11](=[O:12])[CH2:10][CH:9]([C:13]([OH:15])=[O:14])[CH2:8]2)=[CH:3][CH:2]=1.[CH3:17]O.S(=O)(=O)(O)O>C(Cl)Cl>[C:1]1([CH3:16])[CH:2]=[CH:3][C:4]([N:7]2[C:11](=[O:12])[CH2:10][CH:9]([C:13]([O:15][CH3:17])=[O:14])[CH2:8]2)=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 27418271-(4-Methylphenyl)-5-oxopyrrolidine-3-carboxylic acid

생성물 1

HCID 577835HCID 577835, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-(4-Tolyl)-5-oxo-3-pyrrolidinecarboxylic acid (45.50 g) is suspended in methylene chloride (460 ml) and thereto are added methanol (50.5 ml) and conc. sulfuric acid (0.77 ml) and the mixture is refluxed for 19 hours. After cooling, the reaction mixture is concentrated under reduced pressure and the resulting residue is neutralized by adding water and aqueous sodium hydrogen carbonate solution thereto. The precipitated crystal is collected by filtration and washed with water to give the desired product (46.07 g), m.p. 71°-74° C.

후처리

  1. temperaturethe mixture is refluxed for 19 hours
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture is concentrated under reduced pressure
  4. additionby adding water and aqueous sodium hydrogen carbonate solution
  5. filtrationThe precipitated crystal is collected by filtration
  6. washwashed with water

출처 및 근거

ORD 기록
ord-efb1440428bc4feb972b93cda69fe5a1
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05145865

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