HRID322946

反应详情

EQUATION

反应方程式

HRID 322946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6-benzyloxy-1,3-benzoxathiol-2-one (35 g), aqueous sodium hydroxide solution (200 mL; 2 N) and methanol (50 mL) is stirred at ambient temperature for 16 hours and then it is heated at reflux for 30 minutes. The reaction mixture is then evaporated to dryness and the residue is acidified to pH 1 by treatment with concentrated hydrochloric acid (20 mL). The residue is diluted with water (200 mL) and then extracted with diethyl ether (3×200 mL). The combined organic extracts are washed with brine (100 mL), dried over magnesium sulphate, filtered and concentrated in vacuo, to give 5-benzyloxy-2-mercaptophenol, in the form of a yellow oil which solidified on standing overnight.

WORKUP

后处理

  1. temperatureit is heated
  2. temperatureat reflux for 30 minutes
  3. customThe reaction mixture is then evaporated to dryness
  4. additionThe residue is diluted with water (200 mL)
  5. extractionextracted with diethyl ether (3×200 mL)
  6. washThe combined organic extracts are washed with brine (100 mL)
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo