HRID2170927

反应详情

EQUATION

反应方程式

HRID 2170927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

Reaction under argon atmosphere: 3.0 g (15 mmol) of 4-bromo-3,5-dimethylphenol are dissolved in 20.0 ml NMP. 20.0 g (61.4 mmol) of cesium carbonate and 11.0 g (61.0 mmol) of methanesulfonic acid tetrahydropyran-4-yl ester are added. The reaction mixture is stirred at 140° C. for 4 h. The solvent is evaporated. The residue is diluted with EtOAc and washed with water and brine. The organic layer is dried and the solvent is evaporated. The residue is chromatographed on silica gel (CH/EtOAc=99/1→60/40) to give the title compound. Yield: 4.0 g; LC (method 1): tR=1.15 min; Mass spectrum (ESI+): m/z=285 [M+H]+.

WORKUP

后处理

  1. customReaction under argon atmosphere
  2. customThe solvent is evaporated
  3. additionThe residue is diluted with EtOAc
  4. washwashed with water and brine
  5. customThe organic layer is dried
  6. customthe solvent is evaporated
  7. customThe residue is chromatographed on silica gel (CH/EtOAc=99/1→60/40)