HRID1243608

反应详情

EQUATION

反应方程式

HRID 1243608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloro-6-(trifluoromethyl)nicotinonitrile (207 mg) and 1,1-dimethylethyl (3-hydroxypentyl)methylcarbamate (217 mg) were dissolved in dimethylformamide (10 ml) under nitrogen at room temperature. To the resulting solution was added sodium hydride (60% in oil) (80 mg). The solution was then allowed to stir at room temperature under nitrogen for 24 h. The mixture was then poured into water and extracted with diethyl ether three times. The combined organic fractions were washed with brine and then dried (MgSO4). The solvent was evaporated and the residue was purified by chromatography (silica, 25% ethyl acetate/isohexane as eluent) to give 175 mg (45%) of the subtitle compound as an oil.

WORKUP

后处理

  1. extractionextracted with diethyl ether three times
  2. washThe combined organic fractions were washed with brine
  3. dry with materialdried (MgSO4)
  4. customThe solvent was evaporated
  5. customthe residue was purified by chromatography (silica, 25% ethyl acetate/isohexane as eluent)