HRID1905048
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionThe aqueous phase was extracted wih 3×50 ml of CH2Cl2
- dry with materialThe combined extracts were dried (MgSO4)
- filtrationfiltered
- customconc. to yield a solid
- customRecrystallization from heptane