反応 #5429

ord-e8d6c976acfe418eb1c313ed305dfb2d

反応方程式

CCOC(=O)c1nc(SC)sc1C(=O)Cl
4-ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid chloride
CC(C)(C)N
tert-butylamine
Cl
hydrochloric acid
CCOC(=O)c1nc(SC)sc1C(=O)NC(C)(C)C
product
収率 100.2%
CCOC(=O)c1nc(SC)sc1C(=O)NC(C)(C)C
4-Ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid-tert-butylamide
収率 100.2%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the organic phase was separated
  2. 2
    洗浄washed with 50 ml of water
  3. 3
    乾燥dried over sodium sulfate
  4. 4
    その他The solvent was removed under reduced pressure

実験手順

3.50 g (13.2 mmol) of 4-ethoxycarbonyl-2-methylthiothiazole-5-carboxylic acid chloride was dissolved in 20 ml of dichloromethane and dripped, at 0° C., into a solution of 3.20 g (44 mmol) of tert-butylamine in 50 ml of dichloromethane. The mixture was allowed to warm up to room temperature and was then stirred for 14 hours. 100 ml of 10% strength hydrochloric acid was added and the organic phase was separated, washed with 50 ml of water and dried over sodium sulfate. The solvent was removed under reduced pressure, leaving 4.00 g (100%) of product as a yellow crystalline slurry.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05244867uspto-grants-1993_09