反応 #1583887

反応方程式

3-methylpyrrolidin-3-ol hydrochloride

potassium carbonate

diphenylbromomethane

→

1-(diphenylmethyl)-3-methylpyrrolidin-3-ol

収率 52.0%

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   その他After the completion of reaction
2. 2
   その他the resulting mixture was evaporated under reduced pressure
3. 3
   その他to remove acetonitrile
4. 4
   workup.ADDITIONTo the residue was added a mixed solution of dichloromethane and water
5. 5
   抽出for extraction
6. 6
   乾燥The organic phase was dried over anhydrous sodium sulfate
7. 7
   その他evaporated
8. 8
   その他to remove the solvent
9. 9
   その他to produce a crude product
10. 10
    その他The crude product was purified by column chromatography (silica gel column, eluted with petroleum ether:ethyl acetate=30:1 (volumetric ratio))

実験手順

To a reaction flask were added 3-methylpyrrolidin-3-ol hydrochloride (1 g, 7.2 mmol), anhydrous potassium carbonate (2.5 g, 18 mmol) and acetonitrile (50 L). To the resulting mixture was slowly added a solution of diphenylbromomethane (1.78 g, 7.2 mmol) in acetonitrile dropwisely at 85° C. The reaction was conducted for 12 hours. After the completion of reaction monitored by TLC, the resulting mixture was evaporated under reduced pressure to remove acetonitrile. To the residue was added a mixed solution of dichloromethane and water for extraction. The organic phase was dried over anhydrous sodium sulfate and evaporated to remove the solvent to produce a crude product. The crude product was purified by column chromatography (silica gel column, eluted with petroleum ether:ethyl acetate=30:1 (volumetric ratio)) to produce 1-(diphenylmethyl)-3-methylpyrrolidin-3-ol (1 g) in a yield of 52.0%.

出典