반응 #77850

반응 방정식

2,5-dibromopyridine

N-formylpropargylamine

→

title compound 9-1

수율 93.7%

N-(3-{5-[3-(Formamido)prop-1-ynyl]pyridin-2-yl}prop-2-ynyl)formamide

수율 93.7%

용매

diisopropylamine

반응 조건

후처리

1. 1
   온도The mixture was cooled to 20-22° C.
2. 2
   여과filtered
3. 3
   기타The cake was dried
4. 4
   여과The slurry was filtered
5. 5
   기타the cake was dried

실험 절차

A mixture of 2,5-dibromopyridine (100 g), N-formylpropargylamine (87.7 g), PdCl2(PPh3)2 (2.96 g), and CuI (0.2 g) in diisopropylamine (3 L) was heated at 70° C. for 6 h under a nitrogen atmosphere. The mixture was cooled to 20-22° C. and filtered. The cake was dried and then slurried in water (3 L) at 0-5° C. for 3 h. The slurry was filtered, and the cake was dried to afford 95.4 g of the title compound 9-1.

출처