Reaktion #3641

Reaktionsgleichung

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

Lösungsmittel

ethyl alcohol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheating
2. 2
   Temperaturunder reflux for 3 hours
3. 3
   SonstigeThe cooled reaction mixture
4. 4
   Filtrationis filtered through diatomaceous earth
5. 5
   EinengenThe filtrate is concentrated in vacuo to a residue which
6. 6
   workup.DISSOLUTIONis dissolved in methylene chloride
7. 7
   EinengenThe filtrate is concentrated in vacuo

Vorschrift

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.

Quelle