反应详情

温度

100 °C

15 g of compound 45 are dissolved in 100 ml of glacial acetic acid. 7.4 ml of 2-cyanoethylhydrazine are added, and the solution is heated at 100° C. for 2 h. The mixture is added to ice-water and extracted several times with ethyl acetate. The organic phase is extracted with 20% strength ammonium chloride solution and saturated sodium chloride solution and dried over sodium sulfate. 2.40 g of the desired compound 46 crystallize out with the ethyl acetate phase. The mother liquor is concentrated and chromatographed on silica gel (dichloromethane:methanol:glacial acetic acid=100:10:1). A further 1.10 g of compound 46, plus 7.0 g of reisolated precursor 45, are obtained. C17H19N3O3 (313.4); MS (ESI+): 314.2 (M+H)+, tR=0.97 min (Gradient 2).

1. extractionextracted several times with ethyl acetate
2. extractionThe organic phase is extracted with 20% strength ammonium chloride solution and saturated sodium chloride solution
3. dry with materialdried over sodium sulfate
4. custom2.40 g of the desired compound 46 crystallize out with the ethyl acetate phase
5. concentrationThe mother liquor is concentrated
6. customchromatographed on silica gel (dichloromethane:methanol:glacial acetic acid=100:10:1)