HRID1050719

反应详情

EQUATION

反应方程式

HRID 1050719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

3.0 g of ethyl 2,4-dimethylthiazole-5-carboxylate, 7.0 g of ethylamine hydrochloride, 6.0 g of triethylamine, and 100 mL of ethanol were added into a 250 mL of high-pressure reactor. And the reaction mixture was heated to 120-160° C. and stirred for 20 to 30 hours, and then extracted with ethyl acetate, the organic layer was separated while the aqueous layer was extracted with ethyl acetate twice. The organic phases were combined, and dried over anhydrous sodium sulfate after washed with an iced aqueous sodium chloride solution twice, then remove the solvent under reduced pressure to obtain 1.5 g N-ethyl-2,4-dimethylthiazole-5-carboxamide which was used in the next step directly without purification.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customthe organic layer was separated while the aqueous layer
  3. extractionwas extracted with ethyl acetate twice
  4. dry with materialdried over anhydrous sodium sulfate
  5. washafter washed with an iced aqueous sodium chloride solution twice
  6. customremove the solvent under reduced pressure