反应详情

Synthesis was carried out in accordance with the procedure described in U.S. Pat. No. 7,868,199. In a nitrogen atmosphere, 84 g of sodium boron hydride, 1,450 g of diisopropyl ether (IPE), 2,000 g of water and 1.7 g of 25 wt % NaOH aqueous solution were ice cooled, to which 500 g of methyl 3,3,3-trifluoro-2-hydroxy-2-(trifluoromethyl)propanoate was added dropwise. Stirring was continued for 24 hours at room temperature. Under ice cooling, 444 g of 20 wt % hydrochloric acid aqueous solution was added dropwise to quench the reaction. After the water layer was removed, the organic layer was washed with water and concentrated at 50° C. and a slightly reduced pressure of 6.7 kPa, obtaining 682 g of a 61 wt % IPE solution of 3,3,3-trifluoro-2-trifluoromethyl-1,2-propane diol (yield 95%). The compound was used in the subsequent reaction without further purification.

1. customSynthesis
2. additionwas added dropwise
3. customto quench
4. customthe reaction
5. customAfter the water layer was removed
6. washthe organic layer was washed with water
7. concentrationconcentrated at 50° C.