HRID749298

反应详情

EQUATION

反应方程式

HRID 749298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred solution of 1-fluoromethyl-2-phenylethyl methanesulfonate (1.1 g) in anhydrous DMF (15 mL) under nitrogen was added sodium azide (0.53 g) followed by heating at 80° C. overnight. The cooled reaction mixture was diluted with equal parts of water and brine and extracted with EtOAc. The extracts were washed with water and brine, dried over Na2SO4, and concentrated to an oil which was chromatographed over silica gel with a mixture of EtOAc and hexane to give 0.70 g of the title compound. MS ES (M++H−N2) 151.

WORKUP

后处理

  1. customThe cooled reaction mixture
  2. extractionextracted with EtOAc
  3. washThe extracts were washed with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated to an oil which
  6. customwas chromatographed over silica gel with a mixture of EtOAc and hexane