반응 #7545

반응 방정식

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

triethylamine

acetyl chloride

Water

→

N-(1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinyl)acetamide

용매

methylene chloride

ethyl acetate

반응 조건

후처리

1. 1
   기타the organic layer was separated
2. 2
   세척The organic layer was washed with a saturated aqueous sodium chloride solution
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONdistilled under reduced pressure
5. 5
   기타to remove the solvent
6. 6
   기타The residue was purified by a column chromatography (eluent; chloroform:methanol=50:1 to 10:1)

실험 절차

In 5 mL of methylene chloride was dissolved 0.50 g of 1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinamine, and the solution was cooled to −60° C., after which 0.27 mL of triethylamine and 0.14 mL of acetyl chloride were added to the solution and the resulting mixture was stirred at room temperature for 1 hour. Water and ethyl acetate were added to the reaction mixture and the organic layer was separated. The organic layer was washed with 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=50:1 to 10:1) to obtain 0.55 g of N-(1-{3-[2-(1-benzothiophen-5-yl)ethoxy]propyl}-3-pyrrolidinyl)acetamide as a yellow oil.

출처