18677-43-5

基本信息
2,4-Dimthoxypyridine
2,4-DIMETHOXYPYRIDINE
2,4-DimethoxypyridineI
Pyridine, 2,4-dimethoxy-
2,4-Dimethoxypyridine,>98%
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
常見(jiàn)問(wèn)題列表

26452-80-2

124-41-4

18677-43-5
以2,4-二氯吡啶和甲醇鈉為原料合成2,4-二甲氧基吡啶的一般步驟:將新制備的甲醇鈉(24 g,0.44 mol)加入到2,4-二氯吡啶(15 g,0.10 mol)的無(wú)水N-甲基-2-吡咯烷酮(80 mL)溶液中。將反應(yīng)混合物在120℃下攪拌6小時(shí)。反應(yīng)完成后,將混合物冷卻至室溫,用乙酸乙酯(800 mL)稀釋,并用水洗滌。分離有機(jī)層,用無(wú)水硫酸鈉干燥,過(guò)濾后濃縮,得到2,4-二甲氧基吡啶(4),為無(wú)色油狀物,其純度足以用于下一步驟。產(chǎn)量:11.2 g(80%)。1H NMR (400 MHz, DMSO-d6): δ 3.80 (s, 3H), 3.84 (s, 3H), 6.33 (d, J = 2.0 Hz, 1H), 6.60 (dd, J = 2.0 Hz, J = 5.6 Hz, 1H), 7.97 (d, J = 5.6 Hz, 1H); 13C NMR (100 MHz, DMSO-d6): δ 167.5, 165.4, 147.4, 106.1, 93.8, 55.3, 53.1; HRMS (ESI) m/z calcd for C7H10NO2 [M+H]+: 140.0706; found: 140.0707.
參考文獻(xiàn):
[1] Journal of Chemical Research, 2018, vol. 42, # 1, p. 33 - 34
[2] Patent: US2014/94456, 2014, A1. Location in patent: Paragraph 0883-0884
[3] Patent: US2014/94456, 2014, A1. Location in patent: Paragraph 0883-0884
[4] Patent: WO2015/153683, 2015, A1. Location in patent: Paragraph 0677
[5] Recueil des Travaux Chimiques des Pays-Bas, 1950, vol. 69, p. 468,472