Ammonia → HCID 10902369, compound

Temperature

5 °C

To a mixture of 18.5 g (0.1 mol) of cyanuric chloride and 50 mL of acetonitrile was added a mixed solution of 9.9 g (0.1 mol) of cyclohexlamine, 10.1 g (0.1 mol) of triethylamine and 35 mL of water over 2 hours by keeping the reaction temperature not to exceed 5° C. Thereafter, the stirring was continued for 2 hours while maintaining the temperature at 5° C. or lower. Subsequently, 70 mL of an aqueous 28% ammonia solution was dropwise added at the same temperature, followed by stirring at 5° C. for 1 hour, at 20° C. for 1 hour, and at 50° C. for 2 hours. Thereafter, 54.5 g (0.55 mol) of cyclohexylamine was dropwise added at a reaction temperature of 60° C. and the mixture was stirred at 70° C. for 3 hours. To the reaction mixture thus obtained was added 180 g of water, and the mixture was cooled down to 10° C. while continuing the stirring to precipitate crystals, which were collected by filtration, washed 5 times with 80 mL of water, and dried under reduced pressure to obtain 16.5 g (yield 57%) of the titled compound. Melting point: 153° C.

1. customto exceed 5° C
2. waitat 50° C. for 2 hours
3. stirringthe mixture was stirred at 70° C. for 3 hours
4. customTo the reaction mixture thus obtained
5. temperaturethe mixture was cooled down to 10° C.
6. customto precipitate crystals, which
7. filtrationwere collected by filtration
8. washwashed 5 times with 80 mL of water
9. customdried under reduced pressure

ORD record

ord-e554941d53554de48fa33de3fca6b89a

Source dataset

uspto-grants-2000_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06127538