Реакция #3641

Уравнение реакции

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

Растворители

ethyl alcohol

Условия реакции

Обработка

1. 1
   Температураheating
2. 2
   Температураunder reflux for 3 hours
3. 3
   ДругоеThe cooled reaction mixture
4. 4
   Фильтрацияis filtered through diatomaceous earth
5. 5
   КонцентрированиеThe filtrate is concentrated in vacuo to a residue which
6. 6
   workup.DISSOLUTIONis dissolved in methylene chloride
7. 7
   КонцентрированиеThe filtrate is concentrated in vacuo

Методика

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.

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