85231-15-8

基本信息
2,5-二甲基-4-羥基苯甲醛
2,5-dimethyl-4-hydroxybenzaldehyde
4-HYDROXY-2,5-DIMETHYL-BENZALDEHYDE
Benzaldehyde,4-hydroxy-2,5-diMethyl-
制備方法

6745-75-1

85231-15-8
以2,5-二甲基對(duì)茴香醛為原料合成2,5-二甲基-4-羥基苯甲醛的一般步驟: 步驟A: 將4-甲氧基-2,5-二甲基苯甲醛(1.24 g,7.55 mmol)溶解于無(wú)水二氯甲烷(12 mL)中。在攪拌條件下,緩慢滴加純?nèi)寤穑?.75 g,18.5 mmol)。反應(yīng)過(guò)程中觀察到棕褐色沉淀的形成。將所得懸浮液于室溫下持續(xù)攪拌5天。反應(yīng)完成后,將均勻的反應(yīng)混合物小心倒入冰(150 g)中。待冰完全融化后,通過(guò)過(guò)濾分離出固體產(chǎn)物2,5-二甲基-4-羥基苯甲醛,并干燥,得到產(chǎn)物1.28 g(定量收率)。 產(chǎn)物表征數(shù)據(jù):1H-NMR(400 MHz,DMSO-d6)δ= 10.40(s, 1H),9.98(s, 1H),7.54(s, 1H),6.68(s, 1H),3.36(s, 1H),2.49(s, 3H),2.13(s, 3H)。
參考文獻(xiàn):
[1] Patent: WO2007/56366, 2007, A2. Location in patent: Page/Page column 65-66
[2] Patent: WO2007/56496, 2007, A1. Location in patent: Page/Page column 33-34
[3] Patent: WO2007/56497, 2007, A1. Location in patent: Page/Page column 55
[4] Patent: WO2005/51298, 2005, A2. Location in patent: Page/Page column 245
[5] Patent: US2009/28925, 2009, A1. Location in patent: Page/Page column 107