HRID1980605

反应详情

EQUATION

反应方程式

HRID 1980605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

22.2 ml of boron tribromide are added dropwise, under nitrogen and at room temperature, over 15 minutes to a suspension of 39 g of 2-methoxyphenylsulfonamide in 210 ml of dry methylene chloride. The reaction mixture is then stirred for 1 hour at room temperature. After the mixture has been cooled to 0° C., 200 ml of methanol are added over 15 minutes and the clear solution is concentrated. The oily residue is taken up in ethyl acetate and the solution is washed twice with water, dried over sodium sulfate, and evaporated to dryness. The residue is triturated with petroleum ether, affording 25.1 g of 2-hydroxyphenylsulfonamide with a melting point of 136°-138° C.

WORKUP

后处理

  1. temperatureAfter the mixture has been cooled to 0° C.
  2. concentrationthe clear solution is concentrated
  3. washthe solution is washed twice with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated to dryness
  6. customThe residue is triturated with petroleum ether