反应详情

Sodium methoxide (5.4 g., 0.1 mole) and 4-(p-methoxybenzyl)- thiosemicarbazide (2.1 g., 0.1 mole) were stirred in methanol (200 ml.) for a period of five minutes. Ethyl oxamate (11.7 g., 0.1 mole) was then added to the mixture and the resulting mixture was refluxed for a period of three hours. At this point, most of the solvent was evaporated under reduced pressure, water (200 ml.) was added to the residue and the pH adjusted to 2.0 with dilute hydrochloric acid. The resulting solid was then filtered and subsequently dried in vacuo at 50° C. to yield pure 1-oxamoyl-4-(p-methoxybenzyl)-3-thiosemicarbazide (25.7 g., 91% yield), m.p. 185°-190° C.

1. temperaturethe resulting mixture was refluxed for a period of three hours
2. customAt this point, most of the solvent was evaporated under reduced pressure, water (200 ml.)
3. additionwas added to the residue
4. filtrationThe resulting solid was then filtered
5. customsubsequently dried in vacuo at 50° C.