反応 #3636

反応方程式

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

溶媒

ethyl alcohol

反応条件

後処理

1. 1
   温度The mixture is heated
2. 2
   温度under reflux for 3 hours
3. 3
   ろ過the mixture is filtered through diatomaceous earth
4. 4
   濃縮The filtrate is concentrated in vacuo to a residue which
5. 5
   workup.DISSOLUTIONis dissolved in methylene chloride
6. 6
   濃縮The filtrate is concentrated in vacuo

実験手順

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).

出典