반응 #3636

반응 방정식

5,10-dihydro-5-(4-nitrobenzoyl)-4H-pyrazolo-[5,1-c][1,4]benzodiazepine

hydrazine

→

desired product

5,10-Dihydro-5-(4-aminobenzoyl)-4H-pyrazolo-[5,1-c][1,4]benzodiazepine

용매

ethyl alcohol

반응 조건

후처리

1. 1
   온도The mixture is heated
2. 2
   온도under reflux for 3 hours
3. 3
   여과the mixture is filtered through diatomaceous earth
4. 4
   농축The filtrate is concentrated in vacuo to a residue which
5. 5
   workup.DISSOLUTIONis dissolved in methylene chloride
6. 6
   농축The filtrate is concentrated in vacuo

실험 절차

To a solution of 5 mmol of 5,10-dihydro-5-(4-nitrobenzoyl)-4H-pyrazolo-[5,1-c][1,4]benzodiazepine in 25 ml of ethyl alcohol is added 0.3 g of 10% Pd/C and 15 mmol of hydrazine. The mixture is heated under reflux for 3 hours, and the mixture is filtered through diatomaceous earth. The filtrate is concentrated in vacuo to a residue which is dissolved in methylene chloride and passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated in vacuo to give the desired product which is purified by flash chromatography on silica gel to give the desired product as a solid, exact mass by mass spectrometry: 305. 1402 (M+H).

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