HRID1971223

反应详情

EQUATION

反应方程式

HRID 1971223 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1.13 g (7.1 mmol) of 3,4-difluoronitrobenzene (Aldrich, Buchs, Switzerland), 1.04 g (7.81 mmol) of bis(2-methoxyethyl)amine (Fluka, Buchs, Switzerland) and 1.96 g (14.2 mmol) of K2CO3 in 7 ml of DMSO are stirred for 1.5 h at rt and then heated at 80° C. for 4 h. The reaction mixture is quenched with H2O and extracted with EtOAc (2×). The organic layers are washed with brine (3×), dried over MgSO4, filtered and evaporated. The residue is purified by flash chromatography on silica gel (hexane-EtOAc 6:1 to 5:1) to give the title compound as a yellow oil. ES-MS: 273 (M+H)+.

WORKUP

后处理

  1. customThe reaction mixture is quenched with H2O
  2. extractionextracted with EtOAc (2×)
  3. washThe organic layers are washed with brine (3×)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by flash chromatography on silica gel (hexane-EtOAc 6:1 to 5:1)