HRID1605163

反应详情

EQUATION

反应方程式

HRID 1605163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 3.8 g of 8-chloro-1-n-butyl-2,3,4,5-tetrahydro-1-benzazepine-2,5-dione-4-carboxylic acid methyl ester, 1.17 g of 2-aminothiazole and 70 ml of toluene is distilled for 20 hours so that after collecting 25 ml of toluene each, this amount is returned to the reaction mixture. It is finally concentrated to a small volume, the resulting suspension cooled with ice, filtered and the residue recrystallized from chloroform-acetonitrile, to yield the 8-chloro-1-n-butyl-4-(2-thiazolylcarbamoyl)-2,3,4,5-tetrahydro-1-benzazepine-2,5-dione melting at 238° to 240°.

WORKUP

后处理

  1. distillationis distilled for 20 hours so
  2. customthat after collecting 25 ml of toluene each, this amount
  3. concentrationIt is finally concentrated to a small volume
  4. temperaturethe resulting suspension cooled with ice
  5. filtrationfiltered
  6. customthe residue recrystallized from chloroform-acetonitrile