반응 #69798

반응 방정식

2-bromo-5-nitropyridine

morpholine

→

4-(5-Nitropyridin-2-yl)morpholine

수율 95.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도The reaction was refluxed for 4 hr
2. 2
   세척The solution was subsequently washed with saturated aqueous sodium bicarbonate solution and brine
3. 3
   건조The organic layer was dried (Na2SO4)
4. 4
   여과filtered
5. 5
   기타the solvent was removed in vacuo

실험 절차

In a round-bottom flask, to a dichloromethane (125 mL) solution of 2-bromo-5-nitropyridine (5 g, 24.6 mmol), morpholine (5.4 mL, 61.5 mmol) was added. The reaction was refluxed for 4 hr, then cooled to room temperature. The solution was subsequently washed with saturated aqueous sodium bicarbonate solution and brine. The organic layer was dried (Na2SO4), filtered, and the solvent was removed in vacuo. 4-(5-Nitropyridin-2-yl)morpholine, a yellow solid, was obtained: 4.9 g (95% yield); 1H NMR (300 MHz, DMSO) δ 8.95 (d, J=2.7, 1H), 8.22 (dd, J=2.7, 9.6, 1H), 6.92 (d, J=9.6, 1H), 3.74-3.65 (m, 8H); LCMS (M+) m/z 210.34.

출처