反応 #484889

反応方程式

4-(3-aminophenyl)-N-hexyl-4-methylpiperidine

methanesulfonyl chloride

pyridine

→

title compound

収率 136.6%

N-Hexyl-4-(3-methanesulfonylaminophenyl)-4-methylpiperidine

収率 136.6%

ammonia

溶媒

dichloromethane

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   濃縮it was concentrated in vacuo
2. 2
   その他to give the crude product
3. 3
   その他This was purified by silica column chromatography
4. 4
   洗浄eluting with a gradient of ethyl acetate

実験手順

To 4-(3-aminophenyl)-N-hexyl-4-methylpiperidine (Preparation 56, 70.0 mg, 0.27 mmol) in dichloromethane (3 ml) was added methanesulfonyl chloride (61 mg, 0.53 mmol) in dichloromethane (0.5 ml) and pyridine (42 mg, 0.53 mmol) in dichloromethane (0.5 ml) at room temperature. The solution was stirred at room temperature for 16 h, then it was concentrated in vacuo to give the crude product. This was purified by silica column chromatography eluting with a gradient of ethyl acetate:hexane:0.88 ammonia (90:10:1 to 98:2:1) to give the title compound as a colourless oil (65 mg, 72%).

出典