تفاعل #1583882

معادلة التفاعل

3-methylpyrrolidin-3-ol hydrochloride

3-methylpyrrolidin-3-ol hydrochloride

potassium carbonate

2-bromoethylbenzene

→

3-methyl-1-phenylethylpyrrolidin-3-ol

المردود 75.2%

المذيبات

acetonitrile

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   أخرىwas synthesized
2. 2
   أخرىTo a 100 mL reaction flask
3. 3
   أخرىAfter the completion of reaction
4. 4
   أخرىthe resulting mixture was evaporated under reduced pressure
5. 5
   أخرىto remove acetonitrile
6. 6
   workup.ADDITIONTo the residue was added a mixed solution of dichloromethane and water
7. 7
   استخلاصfor extraction
8. 8
   تجفيفThe organic phase was dried over anhydrous sodium sulfate
9. 9
   أخرىevaporated
10. 10
    أخرىto remove the solvent
11. 11
    أخرىto produce a crude product
12. 12
    أخرىThe crude product was purified by column chromatography (silica gel column, eluted with petroleum ether:ethyl acetate=30:1 (volumetric ratio))

الإجراء التجريبي

According to Example 15, 3-methylpyrrolidin-3-ol hydrochloride was synthesized. To a 100 mL reaction flask were added 3-methylpyrrolidin-3-ol hydrochloride (1 g, 7.2 mmol), anhydrous potassium carbonate (2.5 g, 18 mmol) and acetonitrile (15 mL). To the resulting mixture was slowly added a solution of 2-bromoethylbenzene (1.2 g, 6.48 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 3-methyl-1-phenylethylpyrrolidin-3-ol (1 g) in a yield of 75.2%.

المصدر