반응 #3641

반응 방정식

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

hydrazine

→

desired product

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

용매

ethyl alcohol

반응 조건

후처리

1. 1
   온도heating
2. 2
   온도under reflux for 3 hours
3. 3
   기타The cooled reaction mixture
4. 4
   여과is filtered through diatomaceous earth
5. 5
   농축The filtrate is concentrated in vacuo to a residue which
6. 6
   workup.DISSOLUTIONis dissolved in methylene chloride
7. 7
   농축The filtrate is concentrated in vacuo

실험 절차

To a solution of 5 mmol of 9,10-dihydro-10-(4-nitrobenzoyl)-4H-pyrrolo-[1,2-a]thieno[2,3-e][1,4]diazepine in 25 ml of ethyl alcohol is added 0.13 g of 10% Pd/C and 15 mmol of hydrazine followed by stirring and heating under reflux for 3 hours. The cooled reaction 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 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.

출처