反应详情

温度

65 °C

A mixture of 45 g (0.5 mole) carbohydrazide, 84 g NaHCO3 (1.0 mole) and 50 ml methanol was stirred as 114.5 g (1.0 mole) methane sulfonyl chloride was added over 30 minutes. The temperature rose from 25° to 40° C. The stirring was continued for 15 minutes (temp. 44° C). The mixture was then heated to 65° C for two hours, and was then cooled to 25° C and the solid product (including sodium chloride was filtered and washed with methanol and dried. Yield: 146 g. The material was first suspended in water to remove sodium chloride and then filtered, washed with water and dried. Yield: 81 g, m.p. = 207° C dec.

1. additionwas added over 30 minutes
2. customrose from 25° to 40° C
3. custom(temp. 44° C)
4. temperaturewas then cooled to 25° C
5. filtrationwas filtered
6. washwashed with methanol
7. customdried
8. customto remove sodium chloride
9. filtrationfiltered
10. washwashed with water
11. customdried