Reaktion #685003

Reaktionsgleichung

triethylamine

acetyl chloride

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

water

→

yellow oil

N-(1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-3-pyrrolidinyl)acetamide

Lösungsmittel

methylene chloride

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigean organic layer was then separated
2. 2
   WaschenThe organic layer was washed with a saturated saline solution
3. 3
   Trocknendried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONThe solvent was then distilled away under a reduced pressure
5. 5
   SonstigeThe residue was purified by column chromatography (eluent; chloroform:methanol=50:1 to 10:1)

Vorschrift

0.50 g of 1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-3-pyrrolidinamine was dissolved in 5 ml of methylene chloride. The obtained solution was cooled to −60° C. Thereafter, 0.27 ml of triethylamine and 0.14 ml of acetyl chloride were added thereto, and the obtained mixture was stirred at a room temperature for 1 hour. Thereafter, water and ethyl acetate were added to the reaction mixture, and an organic layer was then separated. The organic layer was washed with a saturated saline solution and then dried over anhydrous magnesium sulfate. The solvent was then distilled away under a reduced pressure. The residue was purified by column chromatography (eluent; chloroform:methanol=50:1 to 10:1), so as to obtain 0.55 g of a yellow oil product, N-(1-(3-(2-(1-benzothiophene-5-yl)ethoxy)propyl)-3-pyrrolidinyl)acetamide.

Quelle