HRID1590055

反应详情

EQUATION

反应方程式

HRID 1590055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 58.7 g of 3-hydroxy-2,2-dimethyl-1-propylthiocyanate, 400 ml of acetic anhydride and 400 ml of pyridine was stirred for 16 hours at room temperature. The reaction solution was concentrated under reduced pressure. The residue was dissolved in 500 ml of diethyl ether. The solution was washed in turn with 1N-hydrochloric acid, water, aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous magnesium sulfate. After removing the solvent, the residue was purified by distillation under reduced pressure, thereby affording 53.2 g of 3-acetoxy-2,2-dimethyl-1-propylthiocyanate.

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in 500 ml of diethyl ether
  3. washThe solution was washed in turn with 1N-hydrochloric acid, water, aqueous sodium hydrogen carbonate solution and water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customAfter removing the solvent
  6. distillationthe residue was purified by distillation under reduced pressure