40731-98-4

基本信息
4-羥基-1-茚酮
4-羥基茚酮
4-HYDROXY-INDAN-1-ONE
4-HYDROXYINDANONE
Hydroxyindanone
4-HYDROXY-2,3-DIHYDRO-1H-INDEN-1-ONE
4-HYDROXYINDANONE 98+%
2,3-dihydro-4-hydroxyinden-1-one
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

119-84-6

40731-98-4
以氫化肉桂酸內(nèi)酯為原料合成4-羥基-1-茚酮的一般步驟:將氯化鋁(90.0 g,676 mmol)和氯化鈉的混合物在150℃下攪拌直至固體完全溶解,隨后緩慢滴加氫化肉桂酸內(nèi)酯(20.0 g,135 mmol)。滴加完畢后,將反應(yīng)混合物升溫至200℃并持續(xù)攪拌1小時。反應(yīng)完成后,將混合物冷卻至室溫,并緩慢倒入冰水(500 mL)中,隨后過濾收集粗產(chǎn)物。通過重結(jié)晶純化粗產(chǎn)物,得到4-羥基-1-茚酮(19 g,95%收率),呈灰色固體。該化合物的結(jié)構(gòu)通過以下光譜數(shù)據(jù)確認(rèn):質(zhì)譜(ESI正離子模式)m/z 149.5 [M + H]+;1H NMR(400 MHz,CDCl3)δ(ppm):7.41-7.38(m,1H),7.24-7.19(m,1H),6.80-6.79(m,1H),6.78-6.77(d,1H,J = 4.0 Hz),5.46(br,1H),3.06-3.03(m,2H),2.69-2.66(m,2H)。
參考文獻(xiàn):
[1] Patent: WO2014/19344, 2014, A1. Location in patent: Paragraph 00820
[2] Patent: WO2014/82380, 2014, A1. Location in patent: Paragraph 00314; 00315
[3] Patent: WO2014/82379, 2014, A1. Location in patent: Page/Page column 112; 113
[4] Patent: WO2014/131315, 2014, A1. Location in patent: Page/Page column 112
[5] Patent: US2015/79028, 2015, A1. Location in patent: Paragraph 2389; 2390; 2391; 2392; 2393