反应详情

The product of example 4, step (a) (34 g) was added to a solution of 2-picoline (20 ml) in POCl3 (150 ml) and the mixture refluxed for 24 hr. The reaction mixture was concentrated in vacuo to half its original volume and poured onto ice and then neutralized with ammonia, forming a brown gum. The aqueous phase was decanted off, and the organic residues dissolved in ethyl acetate. This solution was recombined with the aqueous phase, and refluxed for 1 hr. The organic phase was separated, evaporated, and the residue purified by silica gel chromatography, eluting with dichloromethane to afford the subtitled compound as a pale yellow solid (15.6 g).

1. temperaturethe mixture refluxed for 24 hr
2. concentrationThe reaction mixture was concentrated in vacuo to half its original volume
3. additionpoured onto ice
4. customforming a brown gum
5. customThe aqueous phase was decanted off
6. dissolutionthe organic residues dissolved in ethyl acetate
7. temperaturerefluxed for 1 hr
8. customThe organic phase was separated
9. customevaporated
10. customthe residue purified by silica gel chromatography
11. washeluting with dichloromethane