HRID1258697

反应详情

EQUATION

反应方程式

HRID 1258697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-(4-chloro-3-isothiocyanatobenzyl)-1-(trifluoromethyl)cyclopropane carboxamide (0.15 g; 0.45 mmol) and 5-chloro-2-methylamino-4-(4-trifluoromethyl-piperidin-1-yl)aniline (0.14 g; 0.45 mmol) in DMF (3 mL) was stirred overnight at rt. EDC (0.086 g; 0.45 mmol) was added and the mixture was heated to 90° C. for 1 h. The mixture was poured in water, extracted with DCM and the combined organic layer was washed with brine, dried over Na2SO4, filtered, concentrated and purified by column chromatography.

WORKUP

后处理

  1. temperaturethe mixture was heated to 90° C. for 1 h
  2. extractionextracted with DCM
  3. washthe combined organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified by column chromatography