反应详情

To a solution of phenylmethanol (100 μL, 0.965 mmol) in N,N-dimethylformamide (DMF) (8 mL) was added sodium hydride (232 mg, 5.79 mmol) 0° C., the 2-chloro-4-{[2-(4-{[4-chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)ethyl]oxy}-5-fluoropyrimidine (432 mg, 0.965 mmol) was added at 0° C. after 10 min. The reaction mixture was stirred for 30 min, and poured into ice-water (100 mL), extracted with ethyl acetate (50 mL) twice. Combined organic parts were washed with water and brine, dried over sodium sulfate, filtered and concentrated. Purification via ISCO system afforded the title product (370 mg). LC-MS (ESI): m/z 519[M+H]+; 6.26 min (ret time).

1. extractionextracted with ethyl acetate (50 mL) twice
2. washCombined organic parts were washed with water and brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification via ISCO system