[CH3:1][CH:2]([CH3:7])[CH2:3][N+:4]([O-:6])=[O:5].C(=O)([O-])[O-].[K+].[K+].[CH:14](O)([OH:19])[C:15]([F:18])([F:17])[F:16].O>C(OC)(C)(C)C>[CH3:1][CH:2]([CH3:7])[CH:3]([N+:4]([O-:6])=[O:5])[CH:14]([OH:19])[C:15]([F:18])([F:17])[F:16]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.
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