Реакция #352775

Уравнение реакции

2-Hydroxyethyl acrylate

triethylamine

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

→

oil

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

Растворители

diethyl ether

diethyl ether

Условия реакции

Обработка

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

Методика

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).

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