反应详情

温度

0 °C

To a stirred solution of 0.91 g of (4-heptylphenyl)-1,4-diaminoanthraquinone-2-carboxylate (preparation analogous to example 1) in 80 ml of methylenechloride, cooled to 0° C. was added dropwise (over a period of 30 min) a solution of 0.36 g of acryloylchloride in 20 ml of methylenechloride. After stirring for 1 h at 0° C. and 30 min at room temperature, DMAP was added and stirring was continued for further 60 min. The reaction mixture was then concentrated to half its volume and passed through a silica gel column using methylenechloride as the eluent. The afforded violet solid was further recrystallised from ethanol/methylenechloride 9/1 (v/v) to give 0.88 g (4-heptylphenyl)-4-acrylamido-1-aminoanthraquinone-2-carboxylate as violet crystals; λmax. (CB 483): 572 nm.

1. stirringstirring
2. waitwas continued for further 60 min
3. concentrationThe reaction mixture was then concentrated to half its volume
4. customThe afforded violet solid was further recrystallised from ethanol/methylenechloride 9/1 (v/v)