反应详情

39.24 g (0.4 mol) of propiolic acid ethyl ester were added to a solution of 29.63 g (0.4 mol) of N-amino-N-methylformamide in 80 ml of dioxane and left standing for 3 weeks at room temperature. The yellow solution was evaporated at 40° C./30 torr and the residue filtered over a silical gel column (350 g) with a mixture of dichloromethane/n-hexane 49:1 in fractions of 250 ml each. Fractions 2 to 10 were united and evaporated at 40° C./30 torr, yielding 63.9 g (93%) of 3-(formylmethylhydrazono)-propionic acid ethyl ester as a yellow fluid (IR: 3462, 2984, 1735, 1688, 1629, 1183, 1045 cm-1).

1. waitleft
2. waitstanding for 3 weeks at room temperature
3. customThe yellow solution was evaporated at 40° C./30 torr
4. filtrationthe residue filtered over a silical gel column (350 g) with a mixture of dichloromethane/n-hexane 49:1 in fractions of 250 ml each
5. customevaporated at 40° C./30 torr