HRID1094369

反应详情

EQUATION

反应方程式

HRID 1094369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 2-bromo-N-(3,4-dimethyl-phenyl)-N-[2-(6-trifluoromethyl-pyridin-3-yl)-ethyl]-acetamide (134 mg, 0.32 mmol), 2-methylbenzimidazole (85 mg, 0.65 mmol) and potassium carbonate (67 mg, 0.48 mmol) in acetonitrile (1 mL) was irradiated in the microwave for 20 min. at 140° C. The reaction mixture was diluted with TBME (15 mL) and washed with water (15 mL) and brine (15 mL). The aqueous layers were extracted with tert-butylmethylether (15 mL) and the combined organic layers dried over sodium sulfate. Concentration and purification by chromatography (SiO2, heptane:ethyl acetate:methanol=50:50:0 to 0:95:5) afforded the title compound (86 mg, 57%) as a light brown oil. MS m/e: 467.0 [M+H]+.

WORKUP

后处理

  1. customwas irradiated in the microwave for 20 min. at 140° C
  2. washwashed with water (15 mL) and brine (15 mL)
  3. extractionThe aqueous layers were extracted with tert-butylmethylether (15 mL)
  4. dry with materialthe combined organic layers dried over sodium sulfate
  5. concentrationConcentration and purification by chromatography (SiO2, heptane:ethyl acetate:methanol=50:50:0 to 0:95:5)