N-methyl-2-pyrrolidone → 4-Bromo-3-chloro-3,4,4-trifluorobutan-1-ol

Temperature

130 °C

A mixture of 1,4-dibromo-2-chloro-1,1,2-trifluorobutane (XVI) (7.5 g, 24.6 mmol), 1-methyl-2-pyrrolidinone (14 mL) and water (2.5 mL) was heated at 130° C. for 16 hours. The mixture was cooled to room temperature, diluted with water (80 mL) and extracted with ether (2×75 mL). The ether extract was washed with water (3×40 mL), brine, and dried over anhydrous magnesium sulfate. The residue obtained after evaporation of the solvent was chromatographed over silica gel to give 2.9 g (49%) of the desired alcohol as a clear oil.

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ether (2×75 mL)
3. extractionThe ether extract
4. washwas washed with water (3×40 mL), brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe residue obtained
7. customafter evaporation of the solvent
8. customwas chromatographed over silica gel

ORD record

ord-bb9f1dac553247ddb3082b97715ba070

Source dataset

uspto-grants-1997_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05700840