Isopropanol → Isopropyl 4-Methyl-2-thioxopyrrolidine-3-carboxylate

HRID 2372373노트

반응식

HRID 2372373 반응식
[CH3:1][CH:2]1[CH2:6][NH:5][C:4](=[S:7])[CH:3]1[C:8]([O:10][CH2:11][CH3:12])=[O:9].[CH:13](O)(C)C>CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4]>[CH3:1][CH:2]1[CH2:6][NH:5][C:4](=[S:7])[CH:3]1[C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9]

참가 물질

4

반응물 2

HCID 3776IsopropanolHCID 19903350HCID 19903350, 화합물

생성물 1

HCID 10465433Isopropyl 4-Methyl-2-thioxopyrrolidine-3-carboxylate

시약·촉매·용매 1

HCID 11026Titanium isopropoxide촉매

실험 절차

To 5.0 g of ethyl 4-methyl-2-thioxopyrrolidine-3-carboxylate were added 300 ml of isopropyl alcohol and 11.4 g of titanium tetraisopropoxide. The resulting mixture was heated under reflux for 24 hours. After distilling off the excessive isopropyl alcohol 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, 5.0 g of the title compound was obtained.

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 24 hours
  3. distillationAfter distilling off the excessive isopropyl alcohol 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

출처 및 근거

ORD 기록
ord-208e9c7149de4b728082e7eef87488b6
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05098919

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