Ethanol → 1,3-Diazepan-2-one hydrazone hydroiodide

Temperature

-10 °C

A 40.8 gm. (0.15 mole) portion of 2-methylthio-4,5,6,7-tetrahydro-1H-1,3-diazepine hydroiodide in 150 ml. of ethanol is treated with 10 ml. (0.2 mole) of hydrazine hydrate. The solution is stirred at reflux for 3 hours, clarified while hot and then cooled at -10°C. overnight. A 200 ml. portion of ether is added and the mixture is cooled at -10°C. The precipitate is collected, washed with ether and dried at 60°C. under reduced pressure. Yield 20.5 gm., melting point 133°-135°C. Analysis calculated for: C5H12N4 . HI: C, 23.45; H, 5.12; N, 21.88; I, 49.56. Found: C, 22.85; H, 4.96; N, 21.90; I, 50.35.

1. temperatureat reflux for 3 hours
2. temperaturethe mixture is cooled at -10°C
3. customThe precipitate is collected
4. washwashed with ether
5. customdried at 60°C. under reduced pressure

ORD record

ord-811137f5221d47aabe12f5c8a580eb12

Source dataset

uspto-grants-1976_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03931152