HRID512447

反应详情

EQUATION

反应方程式

HRID 512447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Next, a mixture of potassium ethyl xanthate (4.6 g, 28.8 mmol) and crude 2-amino-5-methoxyphenol (4.0 g, 28.8 mmol) was dissolved in ethanol (150 mL). The mixture was heated at 80° C. overnight. After cooling, the solvent was evaporated under reduced pressure. The resultant residue was dissolved in water and treated with 1N HCl to pH 5, resulting in a precipitate, which was collected. The solid thus collected was purified by chromatography with petroleum ether/ethyl acetate (3:1 v/v) to afford 2-mercapto-6-methoxybenzoxazole (4.0 g, yield 77%).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe solvent was evaporated under reduced pressure
  3. dissolutionThe resultant residue was dissolved in water
  4. additiontreated with 1N HCl to pH 5
  5. customresulting in a precipitate, which
  6. customwas collected
  7. customThe solid thus collected
  8. customwas purified by chromatography with petroleum ether/ethyl acetate (3:1 v/v)