Methanol → Methyl 4-(2-oxopyrrolidin-1-yl)benzoate

HRID 1635551노트

반응식

HRID 1635551 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:14][CH2:13][CH2:12][C:11]2=[O:15])=[CH:6][CH:5]=1)([OH:3])=[O:2].S(=O)(=O)(O)O.[CH3:21]O>>[CH3:21][O:2][C:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:14][CH2:13][CH2:12][C:11]2=[O:15])=[CH:6][CH:5]=1)=[O:3]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 7731304-(2-Oxopyrrolidin-1-yl)benzoic acid

생성물 1

HCID 757827Methyl 4-(2-oxopyrrolidin-1-yl)benzoate수율 94%

실험 절차

A mixture of 1-(4-carboxyphenyl)pyrrolidin-2-one (3.0 g, 14.6 mmol) from example 1 and sulfuric acid (0.2 mL) in 100 mL of methanol was stirred at reflux for 18 h. The solvent was removed under vacuum. The crude material was dissolved in 100 mL of ethyl acetate and the solution was washed with a saturated sodium bicarbonate solution (3×15 mL), dried and evaporated to give 3.0 g (94%) of 1-(4-methoxycarbonylphenyl)pyrrolidin-2-one as a white solid, mp 118-120° C. (chloroform/ether).

후처리

  1. temperatureat reflux for 18 h
  2. customThe solvent was removed under vacuum
  3. dissolutionThe crude material was dissolved in 100 mL of ethyl acetate
  4. washthe solution was washed with a saturated sodium bicarbonate solution (3×15 mL)
  5. customdried
  6. customevaporated

출처 및 근거

ORD 기록
ord-667e29fec42d4dad823fe776988d5dde
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06509359B1

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