17802-02-7

物理化學(xué)性質(zhì)
常見問題列表

64182-61-2

17802-02-7
步驟i:將2-氯-6-氟硝基苯(6.62g,37.7mmol)和LiOH·H2O(6.33g,151mmol)溶解于THF(45mL)和水(65mL)的混合溶劑中,隨后加入30% H2O2水溶液(8.60mL,80.0mmol)。將所得混濁溶液密封,在劇烈攪拌下加熱至60℃。反應(yīng)3天后,將深橙色混合物冷卻,加入半飽和硫代硫酸鈉水溶液(200mL),于分液漏斗中劇烈振蕩。隨后,用1N HCl將混合物酸化至pH <3,以EtOAc(400mL + 100mL)萃取,并用鹽水(400mL)洗滌。合并有機(jī)相,用硫酸鎂干燥,過濾后濃縮,得到含有少量固體顆粒(未反應(yīng)的原料)的深黃色油狀物(氨基苯酚10b,6.37g,收率97%),直接用于下一步反應(yīng)。
參考文獻(xiàn):
[1] Patent: WO2009/62285, 2009, A1. Location in patent: Page/Page column 64
[2] Patent: WO2009/62308, 2009, A1. Location in patent: Page/Page column 73-74
[3] Patent: WO2009/62288, 2009, A1. Location in patent: Page/Page column 70-71
[4] Patent: WO2009/62289, 2009, A1. Location in patent: Page/Page column 77-78
[5] Patent: WO2018/37223, 2018, A1. Location in patent: Page/Page column 154