تفاعل #1256707

معادلة التفاعل

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

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling to room temperature
2. 2
   تركيزthe mixture was concentrated in vacuo

الإجراء التجريبي

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.

المصدر