反应详情

EX-632B) To a solution of 4fluorophenol 1.00 g (8.92 mmol) in 30 mL of tetrahydrofuran at 0° C. was added a 60% dispersion of sodium hydride in mineral oil (0.36 g, 8.92 mmol). After 30 min, cyanuric chloride (1.64 g, 8.92 mmol) was added as a heterogeneous mixture in tetrahydrofuran at 0° C. The reaction mixture was allowed to slowly warm to room temperature. After 14 h, the mixture was cooled to 0° C., and a saturated aq. NH4Cl solution was added. The aqueous solution was extracted with diethyl ether (3×50 mL). The combined ether extracts were washed with brine, dried (MgSO4), and concentrated in vacuo to afford 1.34 g (58%) of the desired 2,4-dichloro-6-(4 fluorophenoxy)-1,3,5-triazine product as an off white solid which was taken on to the next step without purification. MS m/z=260 [M+H]+.

1. waitAfter 14 h
2. temperaturethe mixture was cooled to 0° C.
3. extractionThe aqueous solution was extracted with diethyl ether (3×50 mL)
4. washThe combined ether extracts were washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo