158985-25-2

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56621-48-8

24424-99-5

158985-25-2
向4-(1-哌嗪基)苯酚(2.0g,11.22mmol)的水(56mL)溶液中加入氫氧化鈉(673mg,16.83mmol),隨后加入二碳酸二叔丁酯(2.7g,12.34mmol)。將反應(yīng)混合物在室溫下攪拌過夜。次日,過濾反應(yīng)混合物,收集4-(4-羥基苯基)哌嗪-1-甲酸叔丁酯,為褐色固體(3.1g,收率99%),用水(50mL)洗滌后,不經(jīng)進(jìn)一步純化即可用于下一步反應(yīng)。1H NMR(300MHz,DMSO-d6):δ6.79(AA'BB',2H,JAB = 9.1Hz,JAA' = 2.4Hz),6.66(AA'BB',2H,JAB = 9.1Hz,JBB' = 2.4Hz),3.43(dd,4H,J = 5.3,4.9Hz),2.88(dd,4H,J = 5.2,5.1Hz),1.41(s,9H);13C NMR(75.5MHz,DMSO-d6):δ153.8,151.4,144.0,118.5,115.4,78.8,50.3,28.0。
參考文獻(xiàn):
[1] Patent: WO2008/83056, 2008, A2. Location in patent: Page/Page column 51
[2] European Journal of Organic Chemistry, 2009, # 25, p. 4290 - 4299
[3] Bioorganic and Medicinal Chemistry, 2018, vol. 26, # 5, p. 1035 - 1049
[4] ACS Medicinal Chemistry Letters, 2017, vol. 8, # 2, p. 215 - 220
[5] Patent: WO2017/93491, 2017, A1. Location in patent: Page/Page column 3; 12