反应详情

温度

0 °C

Propan-2-ol (785 mg, 13.19 mmol) was added to a solution of chloromethyl chloroformate (1.7 g, 13.19 mmol) in dry ethyl ether (20 mL). The reaction mixture was cooled to 0° C. Pyridine (1.043 g, 13.19 mmol) was added dropwise with stirring. Thereafter, the reaction mixture was stirred at room temperature for 20 hours. The heterogenous mixture was filtered and the filtrate was washed with citric acid 1% (2×20 mL), NaHCO3 1% (2×20 mL) and brine (20 mL). The organic layer was dried over Na2SO4, filtered and evaporated to give desired compound (1.71 g, 85%). 1H NMR (CDCl3) δ: 5.69 (s, 2H, ClCH2O), 4.92 (sept, J=6.26 Hz, 1H, OCH(CH3)2), 1.30 (d, J=6.27 Hz, 6H, OCH(CH3)2). 13C NMR (CDCl3) δ: 152.68, 73.60, 71.95, 21.52 (2C).

1. stirringThereafter, the reaction mixture was stirred at room temperature for 20 hours
2. filtrationThe heterogenous mixture was filtered
3. washthe filtrate was washed with citric acid 1% (2×20 mL), NaHCO3 1% (2×20 mL) and brine (20 mL)
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. customevaporated