2-Methyl-4-isothiazolin-3-one hydrochloride synthesis

Yield:26172-54-3 90 mol %

Reaction Conditions:

in dichloromethane;

Steps:

2 EXAMPLE 2

EXAMPLE 2 A thermometer and dropping funnel were equiped with 1 l three-necked flask, and 3,3'-dithiodipropionamide (23.6 g, 0.1 mol) was dissolved in 350 ml of methylenechloride in the flask. The solution was maintained below 5° C. in cryostat, and herein sulfurylchloride (33.75 g, 0.25 mol) was added dropwise and simultaneously stirred for 3 hr. After stirring at 0° C. for 1 hr, the temperature was slowly increased to room temperature and maintained at 30°+-5° C. in water bath, and then the solution was stirred for 3 hr. The obtained white precipitate was filtered by suction, and then the remaining methylenechloride was removed at 50° C. for 3 hr in vacuum oven to obtain 2-methyl-4-isothiazolin-3-one.HCl (27.4 g, 90 mol %). ¹ H-NMR(100 MHz, D₂ O):δ ppm; 8.53(d, 5H), 6.34(d, 4H), 3.41(s, CH₃)

References:

US5453507,1995,A