反应详情

温度

45 °C

48 g (306 mmol) of benzenecarboximidamide hydrochloride were dissolved in 1.2 l ethanol, and 16.4 ml (337 mmol) of hydrazine hydrate were added. The mixture was stirred at 45° C. for 3 h. 86 g (459 mmol) of ethyl 3-acetamido-2-oxobutanoate (Example 13A), dissolved in 600 ml of ethanol, were added dropwise. The mixture was stirred at 80° C. for another 6 h and at RT for another 12 h. The reaction mixture was chromatographed on silica gel (mobile phase dichloromethane/methanol 20:1). This gave 23.2 g (26% of theory) of the product as a solid.

1. additionwere added dropwise
2. stirringThe mixture was stirred at 80° C. for another 6 h and at RT for another 12 h
3. customThe reaction mixture was chromatographed on silica gel (mobile phase dichloromethane/methanol 20:1)