HRID359778

反应详情

EQUATION

反应方程式

HRID 359778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

22 g of 2-amino-6-(4-fluorophenoxy)benzothiazole (prepared as described in preparation 7) were added to a mixture of a solution of 90 g of potassium hydroxide in 100 ml of water and 28 ml of ethylene glycol, and the mixture was stirred for 2 hours on an oil bath kept at 130° C under an atmosphere of nitrogen. After the mixture had been cooled to room temperature, 90 ml of acetic acid was added dropwise to the resulting homogenous solution to deposit a precipitate: this was extracted with toluene. The toluene extract was dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure, to afford 16 g of the title compound as a pale yellow solid.

WORKUP

后处理

  1. customkept at 130° C under an atmosphere of nitrogen
  2. extractionthis was extracted with toluene
  3. extractionThe toluene extract
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. concentrationconcentrated by evaporation under reduced pressure