反应详情

温度

-20 °C

2-Hydroxyethyl acrylate (11.5 ml, 0.1M) and triethylamine (14.6 ml) in dry diethyl ether (250 ml) were cooled to -25° C. under nitrogen as a solution of 2-chloro-2-oxo-1,3,2-dioxaphospholane (14.3 g) in dry diethyl ether was added over 20 minutes. The mixture was stirred for a further 1 hour at -20° C. and then allowed to warm to 10° C. over a further hour. The precipitate was filtered, washed with ethyl acetate (100 ml) and the combined filtrate and washings evaporated under reduced pressure to give a pale yellow oil (21 g).

1. additionwas added over 20 minutes
2. temperatureto warm to 10° C. over a further hour
3. filtrationThe precipitate was filtered
4. washwashed with ethyl acetate (100 ml)
5. customthe combined filtrate and washings evaporated under reduced pressure