1202577-61-4
1202577-61-4 結(jié)構(gòu)式
基本信息
CYCLOHEXANEMETHANOL, 4-鈥TRIFLUOROMETHYL)鈥鈥 TRANS-
trans-(4-(trifluoromethyl)cyclohexyl)methanol
CYCLOHEXANEMETHANOL, 4-(TRIFLUOROMETHYL)-, TRANS-
物理化學性質(zhì)
制備方法
133261-33-3
1202577-61-4
向氫化鋁鋰(11.6 g,0.306 mol)在無水四氫呋喃(350 mL)中的懸浮液中,于0℃下緩慢滴加反式-4-(三氟甲基)環(huán)己烷甲酸(30 g,0.153 mol)的無水四氫呋喃溶液(50 mL)。反應混合物在0℃下持續(xù)攪拌2小時。通過薄層色譜(TLC,展開劑為石油醚:乙酸乙酯=10:1)監(jiān)測反應進程,確認原料完全消耗。依次用水(12 mL)、15%氫氧化鈉水溶液(24 mL)和水(12 mL)淬滅反應。過濾反應混合物,濾液經(jīng)減壓濃縮,得到反式-(4-(三氟甲基)環(huán)己基)甲醇(24 g,產(chǎn)率86%)為無色液體。產(chǎn)物經(jīng)1H NMR(CDCl3, 400 MHz)表征:δ 3.49-3.50(d, J = 6.0 Hz, 2H),1.91-2.07(m, 4H),1.50-1.57(m, 1H),1.32-1.36(m, 2H),0.98-1.05(m, 2H)。
參考文獻:
[1] Patent: WO2016/61160, 2016, A1. Location in patent: Paragraph 00172
[2] Patent: US2011/53974, 2011, A1. Location in patent: Page/Page column 54
[3] Patent: WO2014/123882, 2014, A1. Location in patent: Page/Page column 82
[4] Patent: WO2017/24018, 2017, A1. Location in patent: Paragraph 00159; 00160
