Hydrochloric Acid → 1,1,1-Trifluoro-2-methyl-2-heptanol

Temperatur

48 °C

24.9 g of trimethyl(trifluoromethyl)silane, 16.0 g of 2-heptanone, 38 g of tetrahydrofuran and 350 mg of tetrabutylammonium fluoride trihydrate were charged into a four-necked flask equipped with a nitrogen feeding tube, a reflux condenser, a dropping funnel and a thermometer, and a reaction was effected by a conventional method. Then, 17.5 g of hydrochloric acid was dropwise added to the reaction mixture at a temperature of 25 to 48° C. over 30 minutes, followed by stirring at about 48° C. for 2 hours. The reaction mixture was treated by a conventional method, and the resulting organic phase was washed with a saline solution, followed by drying with anhydrous magnesium sulfate. Thereafter, the resultant was concentrated under reduced pressure, thereby obtaining 26.4 g of 1,1,1-trifluoro-2-methyl-2-heptanol in the form of a pale brown oily matter.

1. customequipped with a nitrogen feeding tube, a reflux condenser, a dropping funnel
2. additionThe reaction mixture was treated by a conventional method
3. washthe resulting organic phase was washed with a saline solution
4. dry with materialby drying with anhydrous magnesium sulfate
5. concentrationThereafter, the resultant was concentrated under reduced pressure

ORD-Eintrag

ord-4b5604515fcc4a999830feb3f1db4cea

Quelldatensatz

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08105747B2