反应详情

温度

20 °C

Commercially available 2,2-difluoro-1,3-benzodioxole-5-carboxylic acid (1.0 eq) was slurried in toluene (10 vol). Vitride® (2 eq) was added via addition funnel at a rate to maintain the temperature at 15 to 25° C. At the end of the addition, the temperature was increased to 40° C. for 2 hours (h), then 10% (w/w) aqueous (aq) NaOH (4.0 eq) was carefully added via addition funnel, maintaining the temperature at 40 to 50° C. After stirring for an additional 30 minutes (min), the layers were allowed to separate at 40° C. The organic phase was cooled to 20° C., then washed with water (2×1.5 vol), dried (Na2SO4), filtered, and concentrated to afford crude (2,2-difluoro-1,3-benzodioxol-5-yl)-methanol that was used directly in the next step.

1. additionAt the end of the addition
2. temperaturethe temperature was increased to 40° C. for 2 hours (h)
3. temperaturemaintaining the temperature at 40 to 50° C
4. customto separate at 40° C
5. temperatureThe organic phase was cooled to 20° C.
6. washwashed with water (2×1.5 vol)
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated