38267-96-8

基本信息
4-氯-6-溴喹唑啉
6-溴-4-氯喹唑啉 鹽酸鹽
4-Chloro-6-bromoquinazoline
6-Bromo-4-chloroquinazoli...
6-BROMO-4-CHLOROQUINAZOLINE, 95+%
6-Bromo-4-chloro-quinazoline hydrochloride
6-Bromo-4-chloroquinazoline ISO 9001:2015 REACH
物理化學(xué)性質(zhì)
常見問題列表

32084-59-6

38267-96-8
以6-溴-3H-喹唑啉-4-酮(20g,89mmol)為原料合成4-氯-6-溴喹唑啉的一般步驟:將6-溴-3H-喹唑啉-4-酮懸浮于140mL三氯氧磷(POCl3)中,在140℃下攪拌反應(yīng)3小時(shí)。反應(yīng)完成后,將反應(yīng)混合物在真空下濃縮,殘余物溶于500mL二氯甲烷(CH2Cl2)中。用200g固體碳酸氫鈉(NaHCO3)中和反應(yīng)液,過濾后,將濾液在真空下蒸發(fā),得到4-氯-6-溴喹唑啉(21g,收率95%),產(chǎn)物為米色固體。產(chǎn)物經(jīng)1H-NMR(400MHz,CDCl3,298K)表征:δ 7.98(d,1H),8.09(d,1H),8.5(s,1H),9.1(s,1H)。質(zhì)譜(MS)分析顯示:[M + 1]+ m/z 243.0-244.9,保留時(shí)間(Rt)= 1.24分鐘。
參考文獻(xiàn):
[1] Patent: WO2013/57711, 2013, A1. Location in patent: Page/Page column 57
[2] Patent: WO2013/88404, 2013, A1. Location in patent: Page/Page column 186
[3] Patent: US2015/342951, 2015, A1. Location in patent: Paragraph 0974-0975
[4] ACS Medicinal Chemistry Letters, 2016, vol. 7, # 8, p. 762 - 767
[5] Patent: TWI557109, 2016, B. Location in patent: Page/Page column 48; 49; 83