2-硝基苯硼酸頻哪醇酯性質(zhì)、用途與生產(chǎn)工藝
生產(chǎn)方法
以1-溴-2-硝基苯(10.0 g,49.5 mmol,1.0當(dāng)量)和聯(lián)硼酸頻那醇酯(15.08 g,59.4 mmol,1.2當(dāng)量)為原料,加入乙酸鉀(14.57 g,148 mmol,3.0當(dāng)量)和[1,1'-雙(二苯基膦)二氯化鈀(II)](1.09 g,1.49 mmol,0.03當(dāng)量)于二惡烷(180 mL)中。在氮氣保護下,將反應(yīng)混合物于80℃攪拌12小時。反應(yīng)完成后,將混合物減壓濃縮,得到粗產(chǎn)物。通過硅膠柱色譜法(洗脫劑:石油醚/乙酸乙酯,100:1至80:1)純化,得到2-硝基苯硼酸頻哪醇酯,為黃色油狀物(12.0 g,收率97%)。產(chǎn)物經(jīng)1H NMR(DMSO-d6, 400 MHz)鑒定:δ 8.17(d, J = 8.0 Hz, 1H),7.67-7.65(m, 1H),7.58-7.54(m, 2H),1.44(s, 12H)。
參考文獻:
[1] Patent: WO2018/144620, 2018, A1. Location in patent: Paragraph 00334
[2] Advanced Synthesis and Catalysis, 2016, vol. 358, # 6, p. 977 - 983
[3] Synlett, 2018, vol. 29, # 8, p. 1055 - 1060
[4] Journal of the American Chemical Society, 2015, vol. 137, # 21, p. 6738 - 6741
[5] Patent: CN108424344, 2018, A. Location in patent: Paragraph 0083; 0084; 0085; 0095
2-硝基苯硼酸頻哪醇酯
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