反応 #3641

反応方程式

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

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 cooled reaction mixture
4. 4
   ろ過is filtered through diatomaceous earth
5. 5
   濃縮The filtrate is concentrated in vacuo to a residue which
6. 6
   workup.DISSOLUTIONis dissolved in methylene chloride
7. 7
   濃縮The filtrate is concentrated in vacuo

実験手順

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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