反応 #5572

反応方程式

5-[1-(methylsulfonyl)-4-piperidyloxy]-3-nitroimidazo[1,2-a]pyridine

→

desired product

収率 132.6%

3-amino-5-[1-(methylsulfonyl)-4-piperidyloxy]imidazo[1,2-a]pyridine

収率 132.6%

溶媒

methylene chloride

hydrogen

反応条件

後処理

1. 1
   workup.ADDITIONAfter the reaction mixture was treated with Cellite
2. 2
   workup.DISTILLATIONthe solvent was distilled off
3. 3
   workup.ADDITIONTo the residue was added chloroform, which
4. 4
   洗浄was washed in turn with an aqueous saturated sodium bicarbonate solution and water
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONAfter the solvent was distilled off
7. 7
   その他the residue was purified by column chromatography [eluent: chloroform/methanol (15:1)]

実験手順

To a solution of 5-[1-(methylsulfonyl)-4-piperidyloxy]-3-nitroimidazo[1,2-a]pyridine (70 mg, 0.226 mmole) in methylene chloride (10 ml) was added 10% palladium-carbon (50 ml) and the mixture was stirred in hydrogen atmosphere at room temperature for 1.5 hours. After the reaction mixture was treated with Cellite, the solvent was distilled off. To the residue was added chloroform, which was washed in turn with an aqueous saturated sodium bicarbonate solution and water and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography [eluent: chloroform/methanol (15:1)] to obtain 93 mg of the desired product (30.0%, brown oily product).

出典