反応 #5553

反応方程式

5-[4-(amino)butylthio]imidazo[1,2-a]pyridine

triethylamine

methanesulfonyl chloride

→

desired product

収率 50.8%

5-[4-(methanesulfonamido)butylthio] imidazo[1,2-a]pyridine

収率 50.8%

溶媒

methylene chloride

反応条件

後処理

1. 1
   温度cooling
2. 2
   workup.STIRRINGthe mixture was stirred under ice-
3. 3
   温度cooling for 1 hour
4. 4
   洗浄The reaction mixture was washed in turn with an aqueous saturated sodium bicarbonate solution and saturated saline
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: ethyl acetate)

実験手順

To a solution of 5-[4-(amino)butylthio]imidazo[1,2-a]pyridine (440 mg, 1.99 mmoles) and triethylamine (0.42 ml, 3.01 mmoles) in methylene chloride (20 ml) was added methanesulfonyl chloride (0.19 ml, 2.45 mmoles) under ice-cooling with stirring and the mixture was stirred under ice-cooling for 1 hour. The reaction mixture was washed in turn with an aqueous saturated sodium bicarbonate solution and saturated saline and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate) to obtain 302 mg of the desired product (50.8%, light red brown solid).

出典