HCID 19903350、化合物 → HCID 19903323、化合物

HRID 2372372ノート

反応式

HRID 2372372 の反応式
[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]

参加物

4

反応物 1

HCID 19903350HCID 19903350、化合物

生成物 1

HCID 19903323HCID 19903323、化合物収率 52.8%

試薬・触媒・溶媒 2

HCID 11026Titanium isopropoxide触媒HCID 11124Methyl propionate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4298b62038b94fd3be76049365d77d6d
出典データセット
uspto-grants-1992_03
特許番号
US05098919

反応ノート

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