HRID1596309

反应详情

EQUATION

反应方程式

HRID 1596309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 53 mg (0.25 mmol)(2′-methoxy-biphenyl-2-yl)-methyl-amine and 0.064 ml (0.375 mmol) N-ethyldiisopropylamine in 4 ml CH2Cl2 was cooled in an ice bath and a solution of 88 mg (0.275 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride in 1 ml CH2Cl2 was added dropwise. The reaction mixture was stirred overnight at room temperature. Ethyl acetate was added and the organic layer was washed with saturated Na2CO3 solution, 1 N HCl solution, dried (MgSO4) and evaporated. The residue was purified by chromatography (SiO2, hexane/ethyl acetate 4:1) to give 107 mg (87%) 2-(3,5-bis-trifluoromethyl-phenyl)-N-(2′-methoxy-biphenyl-2-yl)-N-methyl-isobutyramide as orange crystals, MS (ISP): 496.1(M+H)+.

WORKUP

后处理

  1. washthe organic layer was washed with saturated Na2CO3 solution, 1 N HCl solution
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customThe residue was purified by chromatography (SiO2, hexane/ethyl acetate 4:1)