反应详情

温度

110 °C

To a solution of 4-amino-5-fluoro-2-methoxybenzonitrile (intermediate 88; 5.3 g, 0.03 mol) in ethanol (20 mL) was added sodium hydroxide 8M (27.9 mL, 0.22 mol), the mixture was placed in a sealed vessel and heated to 110° C. for 20 hours. The solvent was removed under reduced pressure and the crude obtained was partitioned between water and ether. The aqueous layer was acidified by hydrochloric acid 6N until pH 4 and the crude was extracted with ethyl acetate, dried, filtered and evaporated under reduced pressure giving the title compound as a yellow solid (80%), which was used in the next step without further purification.

1. customthe mixture was placed in a sealed vessel
2. customThe solvent was removed under reduced pressure
3. customthe crude obtained
4. customwas partitioned between water and ether
5. extractionthe crude was extracted with ethyl acetate
6. customdried
7. filtrationfiltered
8. customevaporated under reduced pressure