反応 #3631

反応方程式

9,10-dihydro-10-(4-nitrobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine

hydrazine

→

desired product

9,10-Dihydro-10-(4-aminobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine

溶媒

ethyl alcohol

反応条件

後処理

1. 1
   温度heating
2. 2
   温度under reflux for 3 hours
3. 3
   その他The room temperature reaction mixture
4. 4
   ろ過is filtered through diatomaceous earth
5. 5
   濃縮the filtrate concentrated in vacuo
6. 6
   workup.DISSOLUTIONThe residue is dissolved in methylene chloride
7. 7
   濃縮The filtrate is concentrated in vacuo

実験手順

To a solution of 1 mmol of 9,10-dihydro-10-(4-nitrobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine in 20 ml of ethyl alcohol is added 0.2 g of 10% Pd/C and 2.5 mmol of hydrazine followed by stirring and heating under reflux for 3 hours. The room temperature reaction mixture is filtered through diatomaceous earth and the filtrate concentrated in vacuo. The residue 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.

出典