反応 #1001827

反応方程式

methanesulfonyl chloride

Dichloromethane

methyl 9-hydroxynonanoate

pyridine

→

methyl 9-(methanesulfonyloxy)nonanoate

収率 68.0%

溶媒

water

反応条件

後処理

1. 1
   温度gradually warmed to room temperature
2. 2
   workup.STIRRINGstirred for one day
3. 3
   抽出extracted twice with dichloromethane
4. 4
   洗浄The resulting organic layer was washed with 1 N hydrochloric acid and saturated sodium hydrogencarbonate solution
5. 5
   乾燥The organic layer was dried over anhydrous sodium sulfate
6. 6
   その他the solvent was removed
7. 7
   その他The resulting residue was purified by silica gel column chromatography

実験手順

Dichloromethane (20 mL) was added with methyl 9-hydroxynonanoate (2.1 g) and pyridine (1.8 g), stirred at 0° C., added with methanesulfonyl chloride (1.3 mL), gradually warmed to room temperature and stirred for one day. The reaction solution was added with water and then extracted twice with dichloromethane. The resulting organic layer was washed with 1 N hydrochloric acid and saturated sodium hydrogencarbonate solution. The organic layer was dried over anhydrous sodium sulfate, and then the solvent was removed. The resulting residue was purified by silica gel column chromatography to obtain methyl 9-(methanesulfonyloxy)nonanoate (2.1 g, yield: 68%).

出典