反应详情

40 g (1.0 mol) of sodium hydroxide are dissolved in 100 g of water and 200 g of ice in a 1 liter reactor fitted with stirring and cooling means. The sodium hydroxide solution is cooled to 10° C., and 105.1 g (1.0 mol) of aminoacetaldehyde dimethyl acetal and 10 mg of the inhibitor 4hydroxy-2,2,6,6-tetramethylpiperidine 1-oxide are added. 995 g (1.1 mol) of acryloyl chloride are slowly added to this solution at 10° C. over the course of 2 hours. The pH drops slowly and is finally set to pH=7. Amine is no longer present according to GC. The reaction mixture is saturated with sodium chloride and extracted three times with 200 ml of tert-butyl methyl ether. The organic phase is dried, filtered and evaporated on a rotary evaporator. The resultant oil is extracted three times with petroleum ether and subsequently re-dried on a rotary evaporator, giving 130 g of acrylamidoacetaldehyde dimethyl acetal (81% of theory) as an oil. The product is 99% pure according to GC.

1. temperaturecooling means
2. extractionextracted three times with 200 ml of tert-butyl methyl ether
3. customThe organic phase is dried
4. filtrationfiltered
5. customevaporated on a rotary evaporator
6. extractionThe resultant oil is extracted three times with petroleum ether
7. customsubsequently re-dried on a rotary evaporator