반응 #685002

반응 방정식

3-pyrrolidinol

potassium carbonate

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

water

→

achromatic oil

수율 54.2%

1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-3-pyrrolidinol

수율 54.2%

용매

N,N-dimethylformamide

ethyl acetate

반응 조건

후처리

1. 1
   온도After the reaction mixture was cooled
2. 2
   기타an organic layer was separated
3. 3
   세척The organic layer was successively washed with water
4. 4
   건조a saturated saline solution, and then dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONThereafter, the solvent was distilled away under a reduced pressure
6. 6
   기타The residue was purified by column chromatography (eluent; chloroform:methanol=20:1 to 10:1)

실험 절차

1.20 g of 5-(2-(3-chloropropoxy)ethyl)-1-benzothiophene was dissolved in 12 ml of N,N-dimethylformamide. Thereafter, 0.82 g of 3-pyrrolidinol and 1.30 g of potassium carbonate were added to the obtained solution, and the mixture was then stirred at 85° C. for 2.5 hours. After the reaction mixture was cooled, water and ethyl acetate were added thereto, and an organic layer was separated. The organic layer was successively washed with water and a saturated saline solution, and then dried over anhydrous magnesium sulfate. Thereafter, the solvent was distilled away under a reduced pressure. The residue was purified by column chromatography (eluent; chloroform:methanol=20:1 to 10:1), so as to obtain 0.78 g of an achromatic oil product, 1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-3-pyrrolidinol.

출처