反应详情

The product of example 1b above, 2-phenoxy-6-(2,6-difluorophenylamino)benzonitrile, (0.34 g, 1.06 mmol) was dissolved in dry tetrahydrofuran (40 mL) and stirred under argon in a room temperature water bath. Lithium aluminum hydride (0.384 g, 10.1 mmol) was added, and the reaction mixture was heated to 65° C. for 0.5 hour. The reaction mixture was cooled to room temperature and anhydrous sodium sulfate was added followed by quenching by the addition of a freshly prepared saturated solution of anhydrous sodium sulfate. The solvent was evaporated and the residue triturated with ethyl acetate, filtered and evaporated. Flash chromatography on silica gel eluted with 40% methylene chloride/hexane to which 3% methanol was added followed by Gilson hplc purification gave the title compound as a white amorphous solid. mp 113–116° C.

1. temperaturethe reaction mixture was heated to 65° C. for 0.5 hour
2. temperatureThe reaction mixture was cooled to room temperature
3. customby quenching by the addition of a freshly prepared saturated solution of anhydrous sodium sulfate
4. customThe solvent was evaporated
5. customthe residue triturated with ethyl acetate
6. filtrationfiltered
7. customevaporated
8. washFlash chromatography on silica gel eluted with 40% methylene chloride/hexane to which 3% methanol
9. additionwas added
10. customfollowed by Gilson hplc purification