HRID1729628
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- distillationis distilled for 20 hours so
- customthat after collecting 25 ml of toluene each, this amount
- concentrationIt is finally concentrated to a small volume
- temperaturethe resulting suspension cooled with ice
- filtrationfiltered
- customthe residue recrystallized from chloroform-acetonitrile