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物理化學(xué)性質(zhì)
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1153-85-1
以3-溴咔唑和碘苯為起始原料,合成3-溴-N-苯基咔唑的一般步驟如下:在干燥的反應(yīng)燒瓶中,依次加入3-溴-9H-咔唑、碘苯、0.03當(dāng)量的三(二亞芐基丙酮)二鈀(0)(Pd2(dba)3)、0.06當(dāng)量的三丁基膦以及甲苯(0.1M)。將反應(yīng)混合物在室溫下攪拌約12小時。反應(yīng)完成后,將混合物冷卻至環(huán)境溫度,用二氯甲烷進(jìn)行萃取,并用蒸餾水洗滌有機(jī)相。收集有機(jī)相,用無水硫酸鎂(MgSO4)干燥,隨后在減壓下濃縮。殘余物通過柱色譜法純化,得到目標(biāo)產(chǎn)物3-溴-9-苯基-9H-咔唑,收率為87.22%。通過高分辨率質(zhì)譜(HRMS)分析,測得化合物的精確質(zhì)量為321,分子式確認(rèn)為C18H12BrN。
參考文獻(xiàn):
[1] Patent: US2017/162796, 2017, A1. Location in patent: Paragraph 0126; 0127
[2] Patent: KR2015/58973, 2015, A. Location in patent: Paragraph 0106; 0107; 0108
[3] Patent: KR2016/51654, 2016, A. Location in patent: Paragraph 0244-0246
[4] Patent: KR2015/102733, 2015, A. Location in patent: Paragraph 0151-0155
[5] Patent: KR2015/112880, 2015, A. Location in patent: Paragraph 0119; 0120; 0121; 0122; 0123