反应详情

温度

-15 °C

Phytanol (20.0 g, 66.7 mmol), triethylamine (18.6 mL, 133 mmol), and a stir bar were added to a 1000 mL round bottom flask. The flask was sealed and flushed with nitrogen Anhydrous DCM (250 mL) was added, and the mixture cooled to −15° C. (ice and NaCl). Mesyl Chloride (10.4 mL, 133 mmol) was added slowly via syringe over a 30 minute period, and the reaction stirred at −15° C. for a further 1.5 hours. At this point TLC showed that the starting material had been used up. The solution was diluted with DCM (250 mL) and washed with saturated NaHCO3 (2×200 mL). The organic phase was then dried (MgSO4), filtered, and concentrated (rotovap). The crude product was purified by column chromatography. Yield: 21.5 g, 85.7%.

1. customThe flask was sealed
2. customflushed with nitrogen Anhydrous DCM (250 mL)
3. additionwas added
4. washwashed with saturated NaHCO3 (2×200 mL)
5. dry with materialThe organic phase was then dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated (rotovap)
8. customThe crude product was purified by column chromatography