反应详情

To a solution of (1R,2S)-1-[4-(methylsulfonyl)phenyl]-2-amino-3-fluoro-1-propanol (5 g, 0.02 moles) in methylene chloride (100 ml) triethylamine (3.0 g, 0.03 mole) and dichloro acetyl chloride (3.6 g; 0.025 mole) were added at 10–15° C. After completion of reaction in 30 minutes, water (10 ml) was added and layers were separated. Solvent was distilled off from reaction mass, toluene (25 ml) and water (5 ml) were added. The product thus precipitated was filtered, washed with methylene chloride (20 ml) and crystallized from ethanol/water (4:1) to give 5 g of the title compound with purity 99.5% by HPLC.

1. customAfter completion of reaction in 30 minutes
2. customlayers were separated
3. distillationSolvent was distilled off from reaction mass, toluene (25 ml) and water (5 ml)
4. additionwere added
5. customThe product thus precipitated
6. filtrationwas filtered
7. washwashed with methylene chloride (20 ml)
8. customcrystallized from ethanol/water (4:1)