反应详情

Ethoxalyl chloride (10.6 cc) is added dropwise, in the course of 10 minutes, to a solution, at 20° C., of 1-ethyl-thiosemicarbazide (11.9 g) in acetone (200 cc). The temperature rises to 43° C., the mixture is stirred for 1 hour without heating and is concentrated to dryness at 20° C. under 20 mm Hg (2.7 kPa), the residue is taken up in methanol (30 cc) and the crystallisation is started. After filtration and drying, 1-ethyl-1-ethoxalyl-thiosemicarbazide (13.2 g) is obtained in the form of a white solid melting at 170° C.

1. customrises to 43° C.
2. temperaturewithout heating
3. concentrationis concentrated to dryness at 20° C. under 20 mm Hg (2.7 kPa)
4. customthe crystallisation
5. filtrationAfter filtration
6. customdrying