HRID1872784

反应详情

EQUATION

反应方程式

HRID 1872784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 2-amino-3-ethyl-4-trifluoroacetamidophenol (18.15 mmol) and concentrated hydrochloric acid (45 mL) in methanol (5.2 mL) is treated with triethyl orthoformate (27.2 mmol). A simple distillation apparatus is attached and the mixture is heated with an oil bath to 90° C. and methanol is distilled from the reaction. The reaction mixture is cooled to room temperature and distributed between ethyl ether (200 mL) and water (20 mL). The ether layer is washed with a 0.1 M aqueous solution of sodium hydroxide (20 mL), dried over magnesium sulfate and concentrated under reduced pressure to yield 4-ethyl-5-trifluoroacetamidobenzoxazole.

WORKUP

后处理

  1. distillationA simple distillation apparatus
  2. distillationmethanol is distilled from the reaction
  3. temperatureThe reaction mixture is cooled to room temperature
  4. washThe ether layer is washed with a 0.1 M aqueous solution of sodium hydroxide (20 mL)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure