反应详情

温度

0 °C

To a solution of 2-phenoxyethanol (10.0 mL, 80.0 mmol) and triethylamine (13.5 mL, 96.9 mmol) in anhydrous CH2Cl2 (250 mL) at 0° C. is added methanesulfonyl chloride (6.80 mL, 87.9 mmol). The resulting cloudy mixture is stirred at 0° C. for 2 h. The mixture is diluted with water (75 mL) and extracted. The organic layer is washed with 1N HCl (75 mL) then saturated NaHCO3/brine (1:1; 75 mL) dried (Na2SO4), filtered, and concentrated. The residue is dried to constant weight under reduced pressure to provide the title compound as a pale yellow oil (17.1 g, 99%). This material is used in the next step without further purification.

1. extractionextracted
2. washThe organic layer is washed with 1N HCl (75 mL)
3. dry with materialsaturated NaHCO3/brine (1:1; 75 mL) dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue is dried to constant weight under reduced pressure