반응 #1179954

반응 방정식

5-[2-(3-chloropropoxy)ethyl]-1-benzothiophene

3-pyrrolidinol

potassium carbonate

water

→

1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinol

수율 54.2%

용매

N,N-dimethylformamide

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONwere added to the solution
2. 2
   온도After the reaction mixture was cooled
3. 3
   기타the organic layer was separated
4. 4
   세척The organic layer was washed with water
5. 5
   건조a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONdistilled under reduced pressure
7. 7
   기타to remove the solvent
8. 8
   기타The residue was purified by a column chromatography (eluent; chloroform:methanol=20:1 to 10:1)

실험 절차

In 12 mL of N,N-dimethylformamide was dissolved 1.20 g of 5-[2-(3-chloropropoxy)ethyl]-1-benzothiophene, and 0.82 g of 3-pyrrolidinol and 1.30 g of potassium carbonate were added to the solution, after which the resulting mixture was stirred at 85° C. for 2.5 hours. After the reaction mixture was cooled, water and ethyl acetate were added thereto and the organic layer was separated. The organic layer was washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent. The residue was purified by a column chromatography (eluent; chloroform:methanol=20:1 to 10:1) to obtain 0.78 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinol as a colorless oil.

출처