反应详情

温度

0 °C

3-Phenyl-prop-2-yn-1-ol 37 (3.0 g, 22.7 mmol) is dissolved in DCM (50 mL). The solution is cooled to 0° C., then methanesulfonyl chloride (4.5 mL, 34.1 mmol) and triethyl amine (4.7 mL, 34.1 mmol) is added. The mixture is allowed to warm to room temperature and stirred overnight at room temperature. The mixture is washed with H2O (2×30 mL). The organic layer is dried (MgSO4), filtered, and concentrated to afford crude methanesulfonic acid 3-phenyl-prop-2-ynyl ester 38 as a clear oil: 1H-NMR (400 MHz, CDCl3) δ=7.47-7.32 (m, 5H), 4.38 (s, 2H), 3.67 (s, 3H).

1. temperatureto warm to room temperature
2. washThe mixture is washed with H2O (2×30 mL)
3. dry with materialThe organic layer is dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated