반응 #44420

반응 방정식

water

(1S)-1-(3,4-Difluorophenyl)ethanamine

2,6-dichloropyrazine

potassium carbonate

→

pyrazine

수율 35.1%

6-Chloro-N-[(1S)-1-(3,4-difluorophenyl)ethyl]pyrazin-2-amine

수율 35.1%

용매

dioxane

반응 조건

후처리

1. 1
   온도The mixture was then heated
2. 2
   기타The crude reaction mixture
3. 3
   추출extracted with diethyl ether (3×30 mL)
4. 4
   농축The combined organic extracts were concentrated
5. 5
   기타20 g silica cartridge (8:2 petroleum spirits:ethyl acetate, followed by ethyl acetate flush)

실험 절차

(1S)-1-(3,4-Difluorophenyl)ethanamine (977 mg, 6.2 mmol) and 2,6-dichloropyrazine (1.236 g, 8.3 mmol, 1.3 eq) was dissolved in dioxane (5 mL) and potassium carbonate (1.73 g, 2.0 eq) added to the solution. The mixture was then heated at reflux (110° C.) under a nitrogen atmosphere for 65 hours. The crude reaction mixture was then poured onto cold water (30 mL) and extracted with diethyl ether (3×30 mL). The combined organic extracts were concentrated and subjected to flashmaster chromatography (20 g silica cartridge (8:2 petroleum spirits:ethyl acetate, followed by ethyl acetate flush) to afford the desired pyrazine-adduct as an off-white solid (587 mg, 35%).

출처