54840-15-2 4-(Boc-氨基)酚

常温运输。WGK Germany:3。危险等级:IRRITANT。存储类别:11 - 可燃固体。危险性类别:眼部刺激 类别2；经皮刺激 类别2；特异性靶器官毒性-一次接触，类别3。非危险化学品。

化学合成。

化学合成

合成路线 1（1. 合成：54840-15-2）

产率：100% 合成条件：With triethylamine In methanol at 22℃; for 14 h; 实验步骤：向4-氨基苯酚（10.97g，100.5mmol）和三乙胺（30mL）的甲醇（200mL）溶液中加入二碳酸二叔丁酯（24.07g，110.3mmol）。将反应混合物在22℃下搅拌14小时。除去溶剂后，将残余物在乙酸乙酯（250mL）和0.25N盐酸水溶液（100mL）之间分配。分离有机相，用饱和氯化铵水溶液（3×50mL）洗涤，并用无水硫酸钠干燥。除去溶剂，得到白色固体（20.91g，100％收率，ES-（m / z）208.1 [M-H]）。 参考文献：[1] Patent: EP1609789, 2005, A1. Location in patent: Page/Page column 12 [2] Tetrahedron Letters, 2011, vol. 52, # 12, p. 1260 - 1264 [3] Chemical Communications, 2013, vol. 49, # 51, p. 5757 - 5759 [4] Organic Letters, 2016, vol. 18, # 21, p. 5728 - 5731 [5] Comptes Rendus Chimie, 2013, vol. 16, # 11, p. 962 - 966 [6] Tetrahedron Letters, 2006, vol. 47, # 46, p. 8039 - 8042 [7] Patent: US2012/65384, 2012, A1. 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合成路线 2（2. 合成：54840-15-2）

产率：61% 合成条件：With formic acid; oxygen; triethylamine; copper(ll) bromide In acetonitrile at 20℃; for 48 h; UV-irradiation 实验步骤：将N-丁氧基羰基-4-碘苯胺（0.25mmol），溴化铜（0.0375mmol），三乙胺（0.25mmol，1.0当量），HCOOH（0.75mmol，3.0当量）在室温下，120mmol反应溶剂CH₃CN加入到反应管中 在氧气氛下，将混合物在室温下搅拌48小时。用薄层色谱法监测反应完成后，加入20mL水和10mL乙酸乙酯萃取，然后用无水硫酸钠干燥。5分钟后过滤，用乙酸乙酯（5mL×3次）洗涤滤饼，然后旋出溶剂。用柱色谱（洗脱剂：石油醚：乙酸乙酯= 6：1）分离产物，产物呈黄色液体，产率61％; 参考文献：

• [1] Organic Letters, 2018, vol. 20, # 3, p. 708 - 711 [2] Patent: CN107915586, 2018, A. Location in patent: Paragraph 0120-0123