反应详情

温度

20 °C

1.04 ml of triethylamine and then 0.659 g of pyridine-4-carbaldehyde are successively added to a solution of 0.945 g of methyl α-aminoisobutyrate hydrochloride in 28 ml of dichloroethane. The reaction mixture is stirred overnight at a temperature in the region of 20° C. The mixture is purified by filtration on Merck Lichroprep aminopropyl-grafted silica. The filtrate is concentrated under reduced pressure and the residue thus obtained is taken up in 25 ml of methanol, 0.372 g of sodium borohydride is added. The reaction mixture is stirred for 48 hours at a temperature in the region of 20° C. and then poured into a mixture of a normal solution of sodium hydroxide/ice. The mixture obtained is extracted three times with ethyl acetate. The organic phase is dried over magnesium sulfate and then concentrated under reduced pressure. 0.726 g of methyl 2-methyl-2-[(pyrid-4-ylmethyl)amino]propanoate is thus obtained in the form of an oil, the characteristics of which are as follows:

1. filtrationThe mixture is purified by filtration on Merck Lichroprep aminopropyl-grafted silica
2. concentrationThe filtrate is concentrated under reduced pressure
3. customthe residue thus obtained
4. stirringThe reaction mixture is stirred for 48 hours at a temperature in the region of 20° C.
5. customThe mixture obtained
6. extractionis extracted three times with ethyl acetate
7. dry with materialThe organic phase is dried over magnesium sulfate
8. concentrationconcentrated under reduced pressure