HRID1901656

反应详情

EQUATION

反应方程式

HRID 1901656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.4 g of 5-chloro-3-(2-tert-butoxycarbonylamino-3-methylthiocarbamoyloxypropoxy)-1,2-benzoisoxazole in 10 ml of methanol is added 5 ml of a dioxane solution (3.2N) of hydrogen chloride at room temperature, and they are subjected to reaction at the same temperature for three hours, after which the solvent is removed by distillation under reduced pressure. To the residue obtained is added 3 ml of 2-propanol, and the crystals precipitated are collected by filtration, to obtain 0.22 g of pale yellow, crystalline 3-(2-amino-3-methylthiocarbamoyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 198.8°-199.2° C. (decomp.).

WORKUP

后处理

  1. customthey are subjected to reaction at the same temperature for three hours
  2. customafter which the solvent is removed by distillation under reduced pressure
  3. customTo the residue obtained
  4. customthe crystals precipitated
  5. filtrationare collected by filtration