HRID1905048

反应详情

EQUATION

反应方程式

HRID 1905048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,4-Dichloro-5-ethoxycarbonyl-2-methylisothiazolium fluorosulfonate (4.2 g, 0.012 mol) was added to 50 ml of saturated K2CO3 solution. The aqueous phase was extracted wih 3×50 ml of CH2Cl2. The combined extracts were dried (MgSO4), filtered and conc. to yield a solid. Recrystallization from heptane yielded 1.0 g (35%) of 4-chloro-5-ethoxycarbonyl-2-methyl-4-isothiazolin-3-one, mp 142-147. Analysis: Calculated for C7H8ClNO3S; C, 37.92; H, 3.65; Cl, 16.01; N, 6.31; S, 14.47. Found: C, 38.39; H, 3.81; Cl, 15.49; N, 6.31; S, 14.56.

WORKUP

后处理

  1. extractionThe aqueous phase was extracted wih 3×50 ml of CH2Cl2
  2. dry with materialThe combined extracts were dried (MgSO4)
  3. filtrationfiltered
  4. customconc. to yield a solid
  5. customRecrystallization from heptane