Hydrochloric Acid → HCID 178512555, compound

Temperature

87 °C

882 g (747 ml) of 32% hydrochloric acid was added to 1000 g (8.9 mole) of 4-fluoroaniline, the mixture was warmed to 87° C., and 780 ml (9.9 mole) of 50% cyanamide solution was added dropwise thereto over 2 hours. The reaction solution was adjusted to pH 2.4 by adding thereto 120 ml of 32% hydrochloric acid, stirred for 3 hours, and cooled to 60° C. Aqueous sodium carbonate solution (Na2CO3 578 g/water 1640 ml) was added dropwise to the reaction solution over 30 minutes. The reaction mixture was stirred for 40 minutes and then cooled to 15° C. The resulting gray solid product was filtered, washed first with 600 ml of water and then with 2000 ml of ethyl acetate, and finally dried to obtain 1395 g of the title compound, which had a light gray color.

1. additionby adding
2. temperaturecooled to 60° C
3. temperaturecooled to 15° C
4. filtrationThe resulting gray solid product was filtered
5. washwashed first with 600 ml of water
6. dry with materialwith 2000 ml of ethyl acetate, and finally dried

ORD record

ord-3165ecee4cf541b0850b033e241d2d42

Source dataset

uspto-grants-2001_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06252076B1