反应详情

温度

15 °C

The solution of 4-[3-(4-fluorophenoxy)phenyl]-3-butyn-2-ol in methyl t-butyl ether prepared in step 1 was cooled to 0°-10° C. and PBr3 (7.6 kg) was added slowly to maintain the reaction temperature under 15° C. The reaction mixture was agitated for 2 hours and then was quenched by the addition of chilled distilled water (25 kg). The layers were separated and the organic phase was diltuted with methyl t-butyl ether, washed with distilled water and 5% aqueous NaHCO3, and concentrated in vacuo to give 2-bromo-4-[3-(4-fluorophenoxy)phenyl]-3-butyne.

1. customwas quenched by the addition
2. temperatureof chilled
3. distillationdistilled water (25 kg)
4. customThe layers were separated
5. washwashed with distilled water and 5% aqueous NaHCO3
6. concentrationconcentrated in vacuo