HRID1928361

反应详情

EQUATION

反应方程式

HRID 1928361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred and cooled solution of 3-[6′-methyl-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-phenylamine (example 327) (0.400 g, 0.986 mmol) in EtOAc (4 mL) and sat. NaHCO3-sol. (2 mL) was added acetyl chloride (0.080 mL, 1.085 mmol) and the mixture was stirred at 23° C. for 1 h. Diluted with EtOAc, washed with sat. NaHCO3-sol. and water, dried the organic layer over Na2SO4. Removal of the solvent in vacuum left a crude product which was purified by trituration with diethyl ether to give the title compound as a white solid (0.250 g, 57%). MS (ISP) 484.2 [(M+H)+].

WORKUP

后处理

  1. stirringthe mixture was stirred at 23° C. for 1 h
  2. washwashed with sat. NaHCO3-sol
  3. dry with materialand water, dried the organic layer over Na2SO4
  4. customRemoval of the solvent in vacuum
  5. waitleft a crude product which
  6. customwas purified by trituration with diethyl ether