反应详情

A mixture of 2,4-dichloro-6-methoxyquinazoline, (38.3 g, 0.19M assuming 100% yield from previous step), N-methylaniline (19.26 g, 0.18M), sodium acetate (16.4 g, 0.2M) in tetrahydrofuran (2 liters) and water (1 liter) was stirred at room temperature for 8 days. Reaction was then concentrated to low volume (about 500 ml) and an oil separated out which solidified. The solid was filtered off and extracted with dichloromethane. Silica gel column chromatography followed by evaporation to dryness gave a residue which was washed with 40-60° petroleum ether (to remove trace impurity) to yield title compound (31.25 g) m.p. 133°-134°.

1. customReaction
2. concentrationwas then concentrated to low volume (about 500 ml)
3. customan oil separated out which
4. filtrationThe solid was filtered off
5. extractionextracted with dichloromethane
6. customSilica gel column chromatography followed by evaporation to dryness
7. customgave a residue which
8. washwas washed with 40-60° petroleum ether (to remove trace impurity)