7083-19-4
7083-19-4 結(jié)構(gòu)式
物理化學(xué)性質(zhì)
制備方法
613-84-3
74-88-4
7083-19-4
步驟1:將5-甲基水楊醛(2-羥基-5-甲基苯甲醛,CAS號613-84-3)懸浮于5 mL二氯甲烷和5 mL水的混合溶劑中。依次加入1.47 mL(4.4 mmol,3當(dāng)量)1 N氫氧化鈉溶液和1.52 g(2.94 mmol,2當(dāng)量)50%四丁基氫氧化銨水溶液,隨后加入碘甲烷(457 μL,5當(dāng)量)。將反應(yīng)混合物于室溫下攪拌3小時。反應(yīng)完成后,用二氯甲烷萃取反應(yīng)混合物3次,合并有機(jī)相,用飽和食鹽水洗滌,無水硫酸鎂干燥,過濾后減壓濃縮。粗產(chǎn)物通過硅膠快速柱色譜純化(洗脫劑:環(huán)己烷/乙酸乙酯,9/1,v/v),得到215 mg(產(chǎn)率97%)目標(biāo)化合物2-甲氧基-5-甲基苯甲醛。
參考文獻(xiàn):
[1] Canadian Journal of Chemistry, 2012, vol. 90, # 11, p. 965 - 974
[2] Journal of Medicinal Chemistry, 2002, vol. 45, # 19, p. 4188 - 4201
[3] Patent: WO2010/66847, 2010, A1. Location in patent: Page/Page column 70
[4] Indian Journal of Chemistry - Section B Organic Chemistry Including Medicinal Chemistry, 1990, vol. 29, # 9, p. 876 - 878
[5] Beilstein Journal of Organic Chemistry, 2018, vol. 14, p. 734 - 746
