22551-24-2

16630-66-3

22551-24-2

Example 12 Preparation of 2-(methylthio)acetamide (compound of Formula III). 200 g of 2-(methylthio)acetic acid methyl ester was slowly added dropwise to 462.9 g (514.4 mL, 282%) of ammonium hydroxide solution at 20-25°C. The dropwise addition was controlled to be completed within 15 minutes. After the dropwise addition was completed, the reaction mixture was kept at this temperature and continued to be stirred for 2 hours (a white solid precipitated at the beginning of the reaction). Subsequently, the reaction suspension was cooled to 0-5°C and stirring was continued at this temperature for 2 hours to complete crystallization. The white solid product was collected by filtration and the resulting solid was resuspended and treated with 200 mL of 2-propanol for 30 minutes at 0-5 °C. The solid was again filtered, washed with 2-propanol and finally dried under vacuum at 40 °C to give white crystalline 2-(methylthio)acetamide (yield: 76.2%; GC purity: 99.9%).