Ammonia → HCID 178418921, compound

To a solution of sodium acetate trihydrate (5.8 g.) in water (20 ml.) is added 1,1-dibromo-3,3,3-trifluoroacetone (5.9 g., 0.022 mole). The solution is heated 45 minutes at steam bath temperature and then cooled. The solution is added to a solution of 2-methylisonicotinaldehyde (2.4 g., 0.02 mole) in methanol (100 ml.) and concentrated aqueous ammonia (25 ml.). The reaction mixture is allowed to stand 4.5 hours at room temperature. The reaction mixture is concentrated under reduced pressure; an oil separates and solidifies and this is filtered (0.6 g.) after recrystallization from a mixture of water and ethanol to afford 2-methyl-4-pyridyl)-4-trifluoromethylimidazole, m.p., 195°-197° C.

1. temperatureThe solution is heated 45 minutes at steam bath temperature
2. temperaturecooled
3. concentrationThe reaction mixture is concentrated under reduced pressure
4. filtrationan oil separates and solidifies and this is filtered (0.6 g.)
5. customafter recrystallization
6. additionfrom a mixture of water and ethanol

ORD record

ord-ca3e77a4d08844cd961bed2329cc7e8b

Source dataset

uspto-grants-1978_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04125530