反应详情

温度

20 °C

(2,2-difluoro-1,3-benzodioxol-5-yl)-methanol (1.0 eq) is dissolved in MTBE (5 vol). A catalytic amount of DMAP (1 mol %) is added and SOCl2 (1.2 eq) is added via addition funnel. The SOCl2 is added at a rate to maintain the temperature in the reactor at 15-25° C. The temperature is increased to 30° C. for 1 hour then cooled to 20° C. then water (4 vol) is added via addition funnel maintaining the temperature at less than 30° C. After stirring for an additional 30 minutes, the layers are allowed to separate. The organic layer is stirred and 10% (w/v) aq. NaOH (4.4 vol) is added. After stirring for 15 to 20 minutes, the layers are allowed to separate. The organic phase is then dried (Na2SO4), filtered, and concentrated to afford crude 5-chloromethyl-2,2-difluoro-1,3-benzodioxole that is used directly in the next step.

1. temperatureThe temperature is increased to 30° C. for 1 hour
2. temperaturethen cooled to 20° C.
3. temperaturemaintaining the temperature at less than 30° C
4. customto separate
5. stirringThe organic layer is stirred
6. addition10% (w/v) aq. NaOH (4.4 vol) is added
7. stirringAfter stirring for 15 to 20 minutes
8. customto separate
9. dry with materialThe organic phase is then dried (Na2SO4)
10. filtrationfiltered
11. concentrationconcentrated