HRID1459358

反应详情

EQUATION

反应方程式

HRID 1459358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

As described for Example 9, a mixture of 0.377 g (1.44 mmol) of 5-(4-aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine, 0.15 g of triethylamine and 0.300 g (1.44 mmol) of 2-trifluoromethylbenzoyl chloride is stirred at room temperature for 2 hours and then washed with 1N HCl 1M NaHCO3, brine and dried (Na2SO4). The solution is passed through a thin pad of hydrous magnesium silicate and the filtrate evaporated to give a solid. Crystallization from dichloromethanehexane gives 0.41 g of crystals, m.p. 191°-193° C.

WORKUP

后处理

  1. washwashed with 1N HCl 1M NaHCO3, brine
  2. dry with materialdried (Na2SO4)
  3. customthe filtrate evaporated
  4. customto give a solid
  5. customCrystallization from dichloromethanehexane