HRID1406484

反应详情

EQUATION

反应方程式

HRID 1406484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

DIC (1.50 mL, 9.6 mmol) was added to a stirred mixture of 5-[3-(2,6-dichloro-phenyl)-thioureido]-2-fluoro-4-methylamino-benzoic acid ethyl ester (2.70 g, 6.5 mmol) in acetonitrile. After stirring for 1 h the mixture was concentrated i.vac. The residue was taken up in ethanol and 1 M aq. NaOH and stirred for further 40 min at reflux. Ethanol was evaporated, the mixture was diluted with water and filtered. The filtrate was acidified with hydrochloric acid, stirred and filtered. Both residues were combined and dried.

WORKUP

后处理

  1. concentrationwas concentrated i.vac
  2. stirring1 M aq. NaOH and stirred for further 40 min
  3. temperatureat reflux
  4. customEthanol was evaporated
  5. additionthe mixture was diluted with water
  6. filtrationfiltered
  7. stirringstirred
  8. filtrationfiltered
  9. customdried