반응 #156824

반응 방정식

triphenyl phosphite

Methyl 6-((2-methoxy-2-oxoethyl)(methyl)amino)-5-nitronicotinate

hydrogen

→

title compound

수율 68.8%

Methyl 4-methyl-2-oxo-1,2,3,4-tetrahydropyrido[2,3-b]pyrazine-7-carboxylate

수율 68.8%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   온도was then refluxed for 30 min
2. 2
   여과The hot solution was filtered through a pad of celite
3. 3
   세척washed with hot dichloromethane (3×20 mL)
4. 4
   농축The filtrate was concentrated in vacuo

실험 절차

Methyl 6-((2-methoxy-2-oxoethyl)(methyl)amino)-5-nitronicotinate (2.7 g, 9.53 mmol) was dissolved in dichloromethane (10 mL). To the yellow solution was added ammonium metavanadate (30.0 mg, 0.256 mmol), triphenyl phosphite (aprox 30 ul, 0.097 mmol), and Pt/C (300 mg, 5% w/w). The reaction mixture was pressurized with hydrogen gas (110 psi) and stirred at room temperature for 16 h. The reaction was then depressurized and diluted with dichloromethane (100 mL) which was then refluxed for 30 min. The hot solution was filtered through a pad of celite and washed with hot dichloromethane (3×20 mL). The filtrate was concentrated in vacuo to yield the title compound (1.45 g, 68%) as a white solid. [M+H] calc'd for C10H11N3O3, 222; found, 222.

출처