HCID 19903350, 화합물 → HCID 19903323, 화합물

HRID 2372372노트

반응식

HRID 2372372 반응식
[CH3:1][CH:2]1[CH2:6][NH:5][C:4](=[S:7])[CH:3]1[C:8]([O:10][CH2:11]C)=[O:9]>CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4].C(OC)(=O)CC>[CH3:1][CH:2]1[CH2:6][NH:5][C:4](=[S:7])[CH:3]1[C:8]([O:10][CH3:11])=[O:9]

참가 물질

4

반응물 1

HCID 19903350HCID 19903350, 화합물

생성물 1

HCID 19903323HCID 19903323, 화합물수율 52.8%

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 11124Methyl propionate용매

실험 절차

To 4.5 g of ethyl 4-methyl-2-thioxopyrrolidine-3-carboxylate, were added 200 ml of methyl propionate and 7.0 ml of titanium tetraisopropoxide. The resulting mixture was heated under reflux for 3 days. After distilling off the excessive methyl propionate under reduced pressure, water and chloroform were added to the residue and insoluble matters were filtered off. The chloroform layer was washed with water and a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After distilling off the chloroform, ethyl ether was added to the residue to thereby crystallize the same. Thus 2.2 g of the title compound was obtained.

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 3 days
  3. distillationAfter distilling off the excessive methyl propionate under reduced pressure, water and chloroform
  4. additionwere added to the residue and insoluble matters
  5. filtrationwere filtered off
  6. washThe chloroform layer was washed with water
  7. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate
  8. distillationAfter distilling off the chloroform, ethyl ether
  9. additionwas added to the residue
  10. customto thereby crystallize the same

출처 및 근거

ORD 기록
ord-4298b62038b94fd3be76049365d77d6d
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05098919

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