반응 #77844

반응 방정식

2,5-dibromopyridine

N-acetyl-propargylamine

→

1-2

수율 89.7%

N-[3-(5-Bromopyridin-2-yl)prop-2-ynyl]acetamide

수율 89.7%

용매

diisopropylamine

ethyl acetate

반응 조건

후처리

1. 1
   여과The solid was filtered
2. 2
   세척washed with ethyl acetate
3. 3
   세척The filtrate and wash
4. 4
   농축concentrated under reduced pressure
5. 5
   기타The residue was purified by silica gel column chromatography

실험 절차

A mixture of 2,5-dibromopyridine (1-1) (1.19 g), N-acetyl-propargylamine (733 mg), CuI (10 mg), and Pd(PPh3)2Cl2 (73 mg) in diisopropylamine (20 mL) was stirred at ambient temperature under nitrogen atmosphere over 3 days. The mixture was diluted with ethyl acetate (50 mL). The solid was filtered and washed with ethyl acetate. The filtrate and wash were combined and concentrated under reduced pressure. The residue was purified by silica gel column chromatography using ethyl acetate as eluant to give crystalline 1-2 (1.14 g).

출처