Ammonia → 4-Amino-5-bromo-2-chloropyrimidine

2,4-Dichloro-5-bromopyrimidine (200 g, 0.88 mol) is added slowly to NH3 (1000 ml, 7 M in MeOH) while the reaction mixture is kept below 10° C. The reaction mixture is stirred at rt for 2 h, heated to 60° C. for 2 h, and then cooled again to rt and stirred for 55 h. It is concentrated under reduced pressure, and the residue is suspended in H2O (500 ml). The aqueous layer is extracted with EtOAc (3×) and the combined organic layers are dried over MgSO4, filtered, and concentrated under reduced pressure to yield the title compound as a white solid.

1. customis kept below 10° C
2. temperatureheated to 60° C. for 2 h
3. temperaturecooled again to rt
4. stirringstirred for 55 h
5. concentrationIt is concentrated under reduced pressure
6. extractionThe aqueous layer is extracted with EtOAc (3×)
7. dry with materialthe combined organic layers are dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure

ORD record

ord-6f950d2c12e4430a9b5ec705bfdbf1d6

Source dataset

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08420657B2