反应详情

温度

0 °C

To a 250 ml round-bottomed flask, (E)-3-(2-chlorophenyl)prop-2-en-1-ol (2.96 g, 17.5 mmol, Preparation example 1) and Dichloromethane (17.5 ml) were added and the reaction mixture was cooled to 0° C. Diisopropylethylamine (6.1 ml, 35.1 mmol) was added and stirred at 0° C. Methyl chloromethyl ether (2.77 ml, 35.1 mmol) was added dropwise and stirred for overnight. The reaction mixture was quenched with 1N NaOH solution, extracted by dichloromethane. The combined organic extracts were dried over anhydrous magnesium sulfate (MgSO4), filtered and concentrated under vacuum. The crude compound was purified by a silica gel column to produce the title compound (3.43 g, 85˜95%).

1. stirringstirred for overnight
2. customThe reaction mixture was quenched with 1N NaOH solution
3. extractionextracted by dichloromethane
4. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe crude compound was purified by a silica gel column