HRID1729621

反应详情

EQUATION

反应方程式

HRID 1729621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 23.0 g of 8-chloro-1-methyl-2,3,4,5-tetrahydro-1-benzazepine-2,5-dione-4-carboxylic acid methyl ester, 8.9 g of 2-aminothiazole and 360 ml of toluene is distilled for 20 hours so that after collecting 100 ml of toluene each, this amount is returned to the reaction mixture. It is finally concentrated to a volume of 150 ml, the resulting suspension cooled with ice, filtered and the residue recrystallized from chloroform-acetonitrile, to yield the 8-chloro-1-methyl-4-(2-thiazolylcarbamoyl)-2,3,4,5-tetrahydro-1-benzazepine-2,5-dione of the formula ##SPC3##

WORKUP

后处理

  1. distillationis distilled for 20 hours so
  2. customthat after collecting 100 ml of toluene each, this amount
  3. concentrationIt is finally concentrated to a volume of 150 ml
  4. temperaturethe resulting suspension cooled with ice
  5. filtrationfiltered
  6. customthe residue recrystallized from chloroform-acetonitrile