HRID2360515

反应详情

EQUATION

反应方程式

HRID 2360515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.03 g (3-amino-5-tert-butyl-2-methoxy-phenyl)-methanol and 2.4 g imidazole are dissolved in 20 ml of tetrahydrofuran and 2.75 ml trimethylsilyl chloride are added dropwise thereto. The mixture is stirred for 2 hours at ambient temperature, the solvents are eliminated in vacuo and the residue is divided between 10% aqueous potassium carbonate solution and ethyl acetate. The aqueous phase is extracted with ethyl acetate and the combined organic phases are washed with saturated sodium chloride solution. After drying with magnesium sulphate the solvents are eliminated in vacuo and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 95:5 to 50:50).

WORKUP

后处理

  1. extractionThe aqueous phase is extracted with ethyl acetate
  2. washthe combined organic phases are washed with saturated sodium chloride solution
  3. dry with materialAfter drying with magnesium sulphate the solvents
  4. customthe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 95:5 to 50:50)