反应详情

温度

0 °C

Trans-1-diethylphosphonomethoxycyclopent-2-en-4-ol (220 mg, 0.88 mmol) was dissolved in CH2Cl2 (2 mL) and cooled to 0° C. under nitrogen. Triethylamine (192 mg, 192 mmol) was added followed by methanesulphonyl chloride (220 mg, 192 mmol) and the reaction mixture leftto stir for 0.5 hrs at 0° C. The reaction mixture was allowed to warm to room temperature and MeOH was added. The aqueous solution was diluted with CH2Cl2 (10 mL) and washed with water, saturated NaHCO3 and brine. The solution was dried (MgSO4), filtered, concentrated and then purified by flash column chromatography with 5% MeOH/95% CH2Cl2 (144 mg, 62%).

1. temperatureto warm to room temperature
2. washwashed with water, saturated NaHCO3 and brine
3. dry with materialThe solution was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified by flash column chromatography with 5% MeOH/95% CH2Cl2 (144 mg, 62%)