HRID1164107

反应详情

EQUATION

反应方程式

HRID 1164107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride (850 mg) was added slowly to a suspension of 2-hydroxy-3-(o-tolylthio)benzaldehyde (11 g) in methanol (50 ml) at temperature below 15° C., and the mixture was stirred at the same temperature for 15 minutes and then at room temperature for 30 minutes. Methanol was distilled off from the reaction mixture under reduced pressure, and the residue was dissolved in water, acidified with conc. hydrochloric acid and extracted with ethyl acetate. The extract was washed with water, dried and evaporated under reduced pressure. The residue was crystallized with aqueous ethanol to give 2-hydroxy-3-(o-tolylthio)benzyl alcohol (8.45 g), mp. 75°-77° C.

WORKUP

后处理

  1. waitat room temperature for 30 minutes
  2. distillationMethanol was distilled off from the reaction mixture under reduced pressure
  3. dissolutionthe residue was dissolved in water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. customdried
  7. customevaporated under reduced pressure
  8. customThe residue was crystallized with aqueous ethanol