反应详情

A cooled (0° C.) suspension of ethyl 2-chloroacetate (17.47 ml, 163 mmol) and ethyl formate (13.18 ml, 163 mmol) in ether (250 ml) was treated slowly (over 3 hrs) with potassium 2-methylpropan-2-olate (18.31 g, 163 mmol) keeping the temperature below 5° C. The mixture was concentrated in vacuo and the resulting solid was washed with ether and dried (47° C. in a vacuum oven) to afford the title compound; 1H NMR (400 MHz, d6-DMSO) δ 8.95 (1H, s), 3.9 (2H, q), 1.1 (3H, t).

1. temperatureA cooled
2. customthe temperature below 5° C
3. concentrationThe mixture was concentrated in vacuo
4. washthe resulting solid was washed with ether
5. customdried (47° C. in a vacuum oven)