89057-44-3
89057-44-3 結(jié)構(gòu)式
基本信息
5,5,10,10-四甲基二茚
5,10-四甲基茚并[2,1-A]茚
5,5,10,10-四甲基-茚并[2,1-A]茚
5,5,10,10-四甲基-5,10-二氫茚并[2,1-A]茚
1,2,5,10-Tetramethylindeno[2,1-a]indene
5,5,10,10-tetramethyl-Inden[2,1-a]Indene
5,5,10,10-tetramethylindeno[2,1-a]indene
5,5,10,10-TetraMethyl-5,10-dihydroindeno<2,1-a>inden
5,5,10,10-Tetramethyl-5,10-dihydroindeno[2,1-a]indene
Indeno[2,1-a]indene, 5,10-dihydro-5,5,10,10-tetramethyl-
物理化學(xué)性質(zhì)
制備方法
6543-29-9
74-88-4
89057-44-3
在約-78℃條件下,將2.04g(10mmol)5,10-四氫二茚(中間體I-3)和37.5mL(60mmol)正丁基鋰(1.60M己烷溶液)在四氫呋喃中逐漸反應(yīng)。隨后,加入3.8mL(60mmol)碘甲烷,并在室溫下攪拌反應(yīng)混合物約3小時(shí)。反應(yīng)完成后,向混合物中加入5mL 1N鹽酸水溶液以淬滅反應(yīng)。分離有機(jī)相,水相用二氯甲烷(2×100mL)萃取。合并有機(jī)相,用硫酸鎂干燥,隨后蒸發(fā)溶劑。殘余物通過硅膠柱色譜法進(jìn)行分離和純化,得到2.03g 5,10-四甲基二茚(中間體I-4),產(chǎn)率為78%。該化合物通過質(zhì)譜/快原子轟擊質(zhì)譜(MS/FAB)進(jìn)行鑒定。分子式C20H20的計(jì)算分子量為260.37,實(shí)測(cè)值為260.45。
參考文獻(xiàn):
[1] Patent: US2014/27721, 2014, A1. Location in patent: Paragraph 0127; 0131
[2] Patent: KR2016/56315, 2016, A. Location in patent: Paragraph 0197; 0198; 0205; 0206
[3] Patent: US9537104, 2017, B2. Location in patent: Page/Page column 77; 78; 79
[4] Patent: US2017/12205, 2017, A1. Location in patent: Paragraph 0223; 0230;0321
