Hydrochloric Acid → HCID 13317018, compound

2-Chloro-5-methylpyrimidine (5.0 g) was finely powdered and dissolved in dry carbon tetrachloride (250 ml). The solution was treated with dry hydrogen chloride gas to precipitate the hydrochloride salt. The reaction mixture was heated to reflux and illuminated with an internal ultra-violet lamp whilst chlorine was bubbled through the stirred suspension. After 41/2 hours the solution was cooled and filtered and the filtrate concentrated under reduced pressure to give a semi-crystalline residue. The residue was dissolved in ether and filtered and the filtrate concentrated to a colourless oil which on standing gave crystals of 2-chloro-5-trichloromethylpyrimidine (8.9 g).

1. customto precipitate the hydrochloride salt
2. temperatureThe reaction mixture was heated
3. temperatureto reflux
4. customilluminated with an internal ultra-violet lamp whilst chlorine
5. customwas bubbled through the stirred suspension
6. temperatureAfter 41/2 hours the solution was cooled
7. filtrationfiltered
8. concentrationthe filtrate concentrated under reduced pressure
9. customto give a semi-crystalline residue
10. filtrationfiltered
11. concentrationthe filtrate concentrated to a colourless oil which

ORD record

ord-caf2ec8cea6848939bc9e10997eb91a5

Source dataset

uspto-grants-1981_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04248618