2-(Dimethylamino)ethyl acrylate → Quantacure ABQ
反応式
[C:1]([O:5][CH2:6][CH2:7][N:8]([CH3:10])[CH3:9])(=[O:4])[CH:2]=[CH2:3].[Br:11][CH2:12][C:13]1[CH:26]=[CH:25][C:16]([C:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:18])=[CH:15][CH:14]=1>CC(C)=O>[Br-:11].[C:17]([C:16]1[CH:25]=[CH:26][C:13]([CH2:12][N+:8]([CH3:10])([CH3:9])[CH2:7][CH2:6][O:5][C:1](=[O:4])[CH:2]=[CH2:3])=[CH:14][CH:15]=1)(=[O:18])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1参加物
4
実験手順
Dimethylaminoethyl acrylate (9.11 mls) was added to a stirred solution of 4-bromomethylbenzophenone (13.75g) in acetone (50 mls) at 55° C. and the mixture was stirred for two hours at 60°±2° C. After cooling to room temperature, the stirred mixture was further cooled in an ice bath for two hours prior to filtration. After washing the residue with acetone (X1) followed by isopropyl ether (X2) the solid was dried under vacuo at room temperature. The crude title compound was obtained as a white crystalline solid (14.48g; m.p. 121°-123° C.) which was recrystallised from acetone (150 mls). Filtration, followed by sequentially washing with acetone (X1) then isopropyl ether (X1) and drying under vacuo at room temperature gave the title compound (10.26g; yield =49.04%) as white fine granular crystals of melting point equal to 122°-124° C. Analysis: