Acetic Acid → 2-Chloro-5-(trifluoromethyl)pyrimidine

2,4-Dichloro-5-trifluoromethyl-pyrimidine (300 mg, 1.4 mmol), zinc dust (90 mg, 1.4 mmol) and tetrahydrofuran (3 ml) heated to reflux. Acetic acid (0.16 ml, 2.8 mmol) in tetrahydrofuran (3 ml) added dropwise to the mixture over 30 minutes. The resultant mixture was heated for a further 3 hours and then allowed to cool to room temperature and filtered through GF-A paper. The liquors were concentrated and wet with dichloromethane. The mixture was washed with dilute bicarbonate solution and then concentrated in vacuo furnishing a crude material from which the desired target molecule was produced.

1. filtrationfiltered through GF-A paper
2. concentrationThe liquors were concentrated and wet with dichloromethane
3. washThe mixture was washed with dilute bicarbonate solution
4. concentrationconcentrated in vacuo

ORD record

ord-72832cea0d2744548ba9d8c9c42bd5b8

Source dataset

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08796244B2