反应详情

温度

0 °C

The solution from 2-acetoxybenzoic acid (216 mg, 1.2 mmol) in dichloromethane (4 ml) is treated with triethylamine (0.15 ml, 1.2 mmol), cooled to 0° C., treated dropwise with ethyl chloroformate (0.144 ml, 1.0 mmol), stirred at 0° C. for 2 h and filtered. The filtrate is added at room temperature to a solution of 2,2-dimethyl-4-aminomethyl-1,3-dioxolane (293 mg, 1.0 mmol) and triethylamine (0.14 ml) in dichloromethane (4 ml). After 4 h, water (10 ml) is added and the mixture is stirred. The organic phase is washed with dilute hydrochloric acid, saturated aqueous sodium hydrogencarbonate solution and water, dried over magnesium sulphate and concentrated. The residue is purified by column chromatography on silica gel 60 (gradient hexane/ethyl acetate=3/1→1/1). Yield: 143 mg.

1. filtrationfiltered
2. waitAfter 4 h
3. stirringthe mixture is stirred
4. washThe organic phase is washed with dilute hydrochloric acid, saturated aqueous sodium hydrogencarbonate solution and water
5. dry with materialdried over magnesium sulphate
6. concentrationconcentrated
7. customThe residue is purified by column chromatography on silica gel 60 (gradient hexane/ethyl acetate=3/1→1/1)