Ammonia → HCID 18180211, compound

Temperature

160 °C

A suspension of 2-chloro-3-bromo-6-aminopyrazine (15 g, 0.072 mole) in absolute ethanol (150 ml) and 0.880 ammonia (375 ml) was stirred and heated in an autoclave at 160° C. and 20 atm. for 16 hrs The cooled mixture was evaporated in vacuo and extracted with hot methanol (3×100 ml). The combined methanol extracts were evaporated in vacuo. The residue was dissolved in hot chloroform, dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo. The residue was triturated with 40-60° C. petroleum ether, filtered, and dried in vacuo. Yield 5.51 g (40%), M.p. 176-178° C.

1. custom20 atm. for 16 hrs The cooled mixture was evaporated in vacuo
2. extractionextracted with hot methanol (3×100 ml)
3. customThe combined methanol extracts were evaporated in vacuo
4. dissolutionThe residue was dissolved in hot chloroform
5. dry with materialdried over anhydrous magnesium sulphate
6. filtrationfiltered
7. customthe filtrate evaporated in vacuo
8. customThe residue was triturated with 40-60° C. petroleum ether
9. filtrationfiltered
10. customdried in vacuo

ORD record

ord-99f03ff7dba441c99d6dc907edef0e82

Source dataset

uspto-grants-2003_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06599905B2