反应详情

A mixture of 9 g of glycolic acid hydrazide, 7.3 g of methyl isothiocyanate, 50 ml of methanol and 50 ml of ethanol was heated under reflux for 5 hours. Following the addition of 2.3 g of sodium metal, the mixture was further refluxed for 24 hours. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in 150 ml of water and adjusted to pH 2.5 with phosphoric acid. The resultant crystals were collected by filtration and recrystallized from ethanol. By the above procedure there were obtained 5.2 g of the captioned compound. m.p. 199°-201° C.

1. temperaturewas heated
2. temperatureunder reflux for 5 hours
3. temperaturethe mixture was further refluxed for 24 hours
4. concentrationThe reaction mixture was concentrated under reduced pressure
5. dissolutionthe residue was dissolved in 150 ml of water
6. filtrationThe resultant crystals were collected by filtration
7. customrecrystallized from ethanol