反应详情

Methyl-1-methyl-2-(phenylmethylene)hydrazinecarboximidothioate-hydroiodide* (4 g) and triethylamine (2.5 g) were dissolved in dichloromethane (50 ml). To this solution acetyl chloride (1.05 g) was added slowly maintaining temperature below 20° C. The mixture was stirred at room temperature in a dry nitrogen atmosphere for 1.5 h. The organic residues were washed with water (5×20 ml), dried over anhydrous sodium sulphate and the solvent removed in vacuo giving a yellow solid which upon trituration with ether gave the title compound (2.30 g) as an off-white solid of m.pt. 102°-104° C.

1. temperaturemaintaining temperature below 20° C
2. washThe organic residues were washed with water (5×20 ml)
3. dry with materialdried over anhydrous sodium sulphate
4. customthe solvent removed in vacuo
5. customgiving a yellow solid which upon trituration with ether