反应详情

温度

25 °C

A solution of ethyl propiolate (10.0 g, 0.10 mol) in THF (67 mL) was treated dropwise with (trimethylsilyl)diazomethane (51 mL, 0.10 mol) maintaining the temperature between 20-30° C. with ice bath cooling. The mixture was stirred at RT for 4 h then treated cautiously with water (250 mL) with cooling in an ice bath. The organics were evaporated in vacuo and the resulting precipitate was collected by filtration, washed with water and dried at RT in vacuo to give the title compound (13.5 g, 94%). LCMS (Method 3): Rt 2.22 min, m/z 141 [MH+].

1. temperaturecooling
2. temperaturewith cooling in an ice bath
3. customThe organics were evaporated in vacuo
4. filtrationthe resulting precipitate was collected by filtration
5. washwashed with water
6. customdried at RT in vacuo