반응 #1256707

반응 방정식

4

4-(4-methoxy-2,6-dimethyl-phenyl)-3,5-dimethyl-pyridine

iodomethane

→

methyl pyridinium iodide salt

4-(4-methoxy-2,6-dimethyl-phenyl)-1,3,5-trimethyl-pyridinium iodide

용매

CH2Cl2

반응 조건

후처리

1. 1
   온도After cooling to room temperature
2. 2
   농축the mixture was concentrated in vacuo

실험 절차

To a solution of 4 (0.241 g, 1.00 mmol) in dry CH2Cl2 (5 mL) was added dropwise iodomethane (0.32 mL, 0.729 g, 5.10 mmol) at room temperature under N2. The reaction mixture was then refluxed at 60° C. under N2 for 1 h. After cooling to room temperature, the mixture was concentrated in vacuo to give the corresponding methyl pyridinium iodide salt as an analytically pure yellow solid (0.382 g, 99.8%). mp 220-221° C.; 1H NMR (400 MHz, CD2Cl2): δ 9.079 (s, 2H), 6.751 (s, 2H), 4.579 (s, 3H), 3.881 (s, 3H), 2.135 (s, 6H), 1.854 (s, 6H); 13C NMR (100 MHz, CD2Cl2): δ 160.512, 159.866, 143.124, 138.802, 135.527, 125.927, 114.217, 55.692, 48.686, 20.188, 17.331; Anal. Calcd. For C17H22INO: C, 53.27; H, 5.79; N, 3.65. Found: C, 53.15; H, 5.79; N, 3.57.

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