870837-18-6

基本信息
3-methoxy-4-(4-methylimidazole)benzaldehyd
3-methoxy-4-(4-methyl-1-imidazolyl)benzaldehyde
3-METHOXY-4-(4-METHYL-IMIDAZOL-1-YL)-BENZALDEHYDE
3-METHOXY-4-(4-METHYL-1H-IMIDAZOL-1-YL)BENZALDEHYDE
Benzaldehyde, 3-methoxy-4-(4-methyl-1H-imidazol-1-yl)-
物理化學(xué)性質(zhì)
常見問題列表

822-36-6

128495-46-5

870837-18-6
以4-甲基咪唑和3-甲氧基-4-氟苯甲醛為原料合成3-甲氧基-4-(4-甲基-1H-咪唑-1-基)苯甲醛的一般步驟:將4-氟-3-甲氧基苯甲醛(85 g,0.55 mol)、4-甲基-1H-咪唑(90.5 g,1.1 mol)和碳酸銫(268.8 g,0.82 mol)在二甲基甲酰胺(1.7 L)中混合,于100℃下攪拌反應(yīng)1小時(shí)。反應(yīng)完成后,將混合物冷卻至室溫,過濾,濾液經(jīng)減壓濃縮。將濃縮后的殘余物溶解于水(2 L)中,用乙酸乙酯(3×2 L)進(jìn)行萃取。合并有機(jī)層,依次用水和鹽水洗滌,經(jīng)無水硫酸鈉干燥后,減壓濃縮除去溶劑。通過硅膠柱色譜法純化(洗脫劑比例為石油醚:乙酸乙酯=2:1),得到黃色固體。將該固體用乙酸乙酯(300 mL)重結(jié)晶,得到白色固體狀的3-甲氧基-4-(4-甲基-1H-咪唑-1-基)苯甲醛。產(chǎn)量:17.8 g,0.082 mol,收率15%。1H NMR(300 MHz,CDCl3)δ 2.31(d,J = 1.0 Hz,3H),3.97(s,3H),7.01(m,1H),7.45(d,J = 7.8 Hz,1H),7.54-7.58(m,2H),7.83(d,J = 1.3 Hz,1H),10.01(s,1H)。
參考文獻(xiàn):
[1] Patent: WO2010/100606, 2010, A1. Location in patent: Page/Page column 41-42
[2] Bioorganic and Medicinal Chemistry Letters, 2011, vol. 21, # 2, p. 773 - 776
[3] Bioorganic and Medicinal Chemistry Letters, 2011, vol. 21, # 13, p. 4083 - 4087
[4] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 9, p. 3140 - 3146
[5] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 9, p. 3140 - 3146