24188-78-1

物理化學(xué)性質(zhì)
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77077-83-9

24188-78-1
步驟2:將4-甲基-2H-異喹啉-1-酮(4.8 g)溶于三氯氧磷(50 mL)中,加熱回流3小時。反應(yīng)完成后,冷卻至室溫并減壓濃縮。殘余物用5 N氫氧化鈉水溶液處理,隨后用二氯甲烷萃取。合并有機層,用飽和食鹽水洗滌,無水硫酸鎂干燥。過濾后,濾液減壓濃縮,所得粗產(chǎn)物通過Biotage快速色譜法純化,洗脫劑為5%乙酸乙酯的己烷溶液,得到4.8 g(收率90%)目標(biāo)產(chǎn)物1-氯-4-甲基異喹啉,為白色固體。產(chǎn)物結(jié)構(gòu)經(jīng)1H NMR(400 MHz,CDCl3)確認(rèn):δ 2.59(s,3H),7.68(t,J = 7.70 Hz,1H),7.78(m,1H),7.94(d,J = 8.31 Hz,1H),8.11(s,1H),8.35(d,J = 8.31 Hz,1H)。
參考文獻:
[1] Patent: US2006/183694, 2006, A1. Location in patent: Page/Page column 73-74
[2] Patent: WO2003/99274, 2003, A1. Location in patent: Page 324-325
[3] Patent: US2007/99825, 2007, A1. Location in patent: Page/Page column 62
[4] Patent: US2008/107623, 2008, A1. Location in patent: Page/Page column 57
[5] Patent: US2008/107624, 2008, A1. Location in patent: Page/Page column 60