HRID2097282

反应详情

EQUATION

反应方程式

HRID 2097282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(2,4-Bis-benzyloxy-5-tert-butyl-phenyl)-isoxazole-3-carboxylic acid ethyl ester (10.0 g, 20.6 mmol) was added to a solution of ethylamine in methanol (60 ml, 2.0M) and the suspension heated, oil bath temperature 75° C., for ˜2 hrs. The resulting solution was allowed to cool and concentrated to a pale brown oil, dichloromethane (150 ml) was added and the solution washed with water (100 ml) and saturated aqueous sodium chloride solution (75 ml). The solution was dried over anhydrous sodium sulphate and concentrated to a brown oil, solidified on standing (9.9 g, ˜quant).

WORKUP

后处理

  1. temperaturethe suspension heated
  2. temperatureto cool
  3. concentrationconcentrated to a pale brown oil, dichloromethane (150 ml)
  4. additionwas added
  5. washthe solution washed with water (100 ml) and saturated aqueous sodium chloride solution (75 ml)
  6. dry with materialThe solution was dried over anhydrous sodium sulphate
  7. concentrationconcentrated to a brown oil