75416-51-2

基本信息
8-bromo-1,2,3,4-tetrahydroisoquinoline
Isoquinoline, 8-broMo-1,2,3,4-tetrahydro-
Isoquinoline, 8-bromo-1,2,3,4-tetrahydro-, hydrochloride (1:1)
物理化學(xué)性質(zhì)
制備方法

252331-63-8

726136-49-8

226942-29-6

75416-51-2
向甲醇(20 mL)和飽和碳酸鈉水溶液(20 mL)的混合溶劑中加入1-(6-溴-3,4-二氫異喹啉-2(1H)-基)-2,2,2-三氟乙酮與1-(8-溴-3,4-二氫異喹啉-2(1H)-基)-2,2,2-三氟乙酮的混合物(3 g,9.7 mmol)。將反應(yīng)混合物加熱回流過夜,隨后濃縮。殘余物用二氯甲烷萃取,合并有機(jī)層,依次用水和飽和氯化鈉溶液洗滌,無水硫酸鈉干燥,減壓蒸除溶劑。粗產(chǎn)物通過硅膠柱色譜(230-400目)純化,以0-2%甲醇/氯仿溶液為洗脫劑,依次得到8-溴-1,2,3,4-四氫異喹啉(第一餾分,無色粘性油狀物,0.45 g,收率22%)和6-溴-1,2,3,4-四氫異喹啉(第二餾分,白色固體,1.0 g,收率48%)。質(zhì)譜(MS)m/z: 211.9 [M + H]+。
參考文獻(xiàn):
[1] Patent: WO2008/76954, 2008, A2. Location in patent: Page/Page column 50
[2] Patent: US2008/171754, 2008, A1. Location in patent: Page/Page column 101; 102
[3] Patent: WO2009/39134, 2009, A1. Location in patent: Page/Page column 179
[4] Patent: WO2006/65215, 2006, A1. Location in patent: Page/Page column 17; 24
[5] Patent: WO2006/65216, 2006, A1. Location in patent: Page/Page column 16; 24