HRID2069269

反应详情

EQUATION

反应方程式

HRID 2069269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 240 mg (0.90 mmol) of 5-fluoro-2-nitro-4-trifluoromethyl-benzoic acid methyl ester and 0.189 ml (2.00 mmol) of thiomorpholine in 2.5 ml of tetrahydrofuran is heated at reflux for 2 hours. After evaporation of the tetrahydrofuran the residue is distributed between water and ethyl acetate, the organic phase separated and washed with water and brine, dried over Na2SO4 and concentrated yielding 310 mg of 2-nitro-5-thiomorpholin-4-yl-4-trifluoromethyl-benzoic acid methyl ester as brown powder, m.p. 68-82° C.

WORKUP

后处理

  1. temperatureat reflux for 2 hours
  2. customAfter evaporation of the tetrahydrofuran the residue
  3. customthe organic phase separated
  4. washwashed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated