反应详情

105.5 g (1.01 mol) of methacryloyl chloride were added dropwise between -30° and -35° C. to a stirred solution of 160 g (1.01 mol) of N-formyl-N-'-2-hydroxyethylpiperazine, 111 g (1.10 mol) of triethylamine and 100 mg of 2,6-di-tert.-butyl-4-methylphenol in 300 ml of dichloromethane and the mixture was stirred for two hours at the same temperature. The precipitate which deposited was filtered off and the filtrate was washed with sodium chloride solution, dried and concentrated to give 166.8 g (73% of theory) of a clear oil of N-formyl-N'-(methacryloyloxyethyl)piperazine. It was possible to elute this with methanol in high purity from a silica gel column after separating small amounts of by-products with ether/n-hexane (6:4).

1. filtrationThe precipitate which deposited was filtered off
2. washthe filtrate was washed with sodium chloride solution
3. customdried
4. concentrationconcentrated