反应详情

温度

20 °C

2.89 g (2.81 ml, 57.73 mmol) of hydrazine hydrate are added dropwise to 9.70 g (48.11 mmol) of 3-nitrobenzenecarboximidamide hydrochloride from example 2A in 200 ml of ethanol. The mixture is stirred for one hour at 20° C. After this time, 13.51 g (72.17 mmol) of ethyl 3-(acetylamino)-2-oxobutanoate from example 4A are added in ethanol, and the reaction mixture is stirred for 4 h at a bath temperature of 70–80° C., subsequently for 12 h at 20° C. The mixture is concentrated and the residue is purified by flash chromatography (eluent: ethyl acetate, subsequently dichloromethane/methanol 30:1).

1. stirringthe reaction mixture is stirred for 4 h at a bath temperature of 70–80° C.
2. waitsubsequently for 12 h at 20° C
3. concentrationThe mixture is concentrated
4. customthe residue is purified by flash chromatography (eluent