反应详情

温度

15 °C

3A Molecular sieves (27.04 g) were heated at 120° C. under vacuum for 20 hours and added to a solution of 2-methyl-1-nitropropane (13.0 g) in methyl tert-butyl ether (420 ml). The mixture was stirred for 5 minutes, potassium carbonate (64.5 g) added and the mixture stirred a further 30 minutes. The mixture was cooled to 15° C. and fluoral hydrate (22.0 g) was added over 30 minutes. The reaction mixture was stirred at ambient temperature for 16 hours, then cooled to 15° C. and water (270 ml) added. After stirring for 5 minutes at ambient temperature, the organic phase was separated and washed with 10% aqueous potassium carbonate, 2M hydrochloric acid solution and water. Solvent was then removed by evaporation under reduced pressure at a temperature below 40° C. and the oil azeotroped dry with isopropyl alcohol at a temperature below 50° C. to give 4-methyl-3-nitro-1,1,1-trifluoro-2-pentanol (21.3 g) as an oil, which was used without further purification.

1. stirringthe mixture stirred a further 30 minutes
2. stirringThe reaction mixture was stirred at ambient temperature for 16 hours
3. temperaturecooled to 15° C.
4. stirringAfter stirring for 5 minutes at ambient temperature
5. customthe organic phase was separated
6. washwashed with 10% aqueous potassium carbonate, 2M hydrochloric acid solution and water
7. customSolvent was then removed by evaporation under reduced pressure at a temperature below 40° C.
8. customthe oil azeotroped
9. dry with materialdry with isopropyl alcohol at a temperature below 50° C.