반응 #352775

반응 방정식

2-Hydroxyethyl acrylate

triethylamine

2-chloro-2-oxo-1,3,2-dioxaphospholane

→

oil

2-(2-Oxo-1,3,2-dioxaphospholan-2-yloxy)ethyl acrylate

용매

diethyl ether

diethyl ether

반응 조건

후처리

1. 1
   workup.ADDITIONwas added over 20 minutes
2. 2
   온도to warm to 10° C. over a further hour
3. 3
   여과The precipitate was filtered
4. 4
   세척washed with ethyl acetate (100 ml)
5. 5
   기타the combined filtrate and washings evaporated under reduced pressure

실험 절차

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).

출처