Methanol → HCID 13772856, 화합물

HRID 344229노트

반응식

HRID 344229 반응식
[C:1]1([C@@H:7]([N:9]2[C:13](=[O:14])[CH2:12][C@H:11]([C:15]([OH:17])=[O:16])[CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.[CH3:23]O>>[C:1]1([C@@H:7]([N:9]2[C:13](=[O:14])[CH2:12][C@H:11]([C:15]([O:17][CH3:23])=[O:16])[CH2:10]2)[CH3:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 723630(3S)-5-oxo-1-[(1S)-1-phenylethyl]pyrrolidine-3-carboxylic acid

생성물 1

HCID 13772856HCID 13772856, 화합물

실험 절차

(3S)-1-((S)-1-Phenylethyl)-5-oxo-3-pyrrolidinecarboxylic acid (666 g, optical purity not less than 99%) was dissolved in methanol (6 l), and conc. sulfuric acid (15 ml) was added at room temperature. The mixture was stirred at refluxing temperature for 7 hr. Methanol was evaporated, and the residue was extracted with ethyl acetate. The organic layer was washed with sodium hydrogencarbonate, dried over magnesium sulfate and concentrated under reduced pressure to give 738 g of methyl (3S)-1-((S)-1-phenylethyl)-5-oxo-3-pyrrolidine-carboxylate.

후처리

  1. temperatureat refluxing temperature for 7 hr
  2. customMethanol was evaporated
  3. extractionthe residue was extracted with ethyl acetate
  4. washThe organic layer was washed with sodium hydrogencarbonate
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-737d2879531445e9bf38f47de4c0651f
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05864039

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