478841-10-0

基本信息
叔丁基 3-羥基高哌啶-1-甲酸
3-羥基氮雜環(huán)庚烷-1-羧酸叔丁酯
3-羥基氮雜環(huán)庚烷-1-甲酸叔丁酯
1H-Azepine-1-carboxylic acid, hexahydro-3-hydroxy-, 1,1-dimethylethyl ester
物理化學(xué)性質(zhì)
常見問題列表

870842-23-2

478841-10-0
以N-Boc-3-氮雜環(huán)庚酮為原料合成3-羥基氮雜環(huán)庚烷-1-甲酸叔丁酯的一般步驟:在0℃下,向N-Boc-3-氮雜環(huán)庚酮(5.5g,25.8mmol)的甲醇(55mL)溶液中分批加入硼氫化鈉(NaBH4)(0.98g,25.8mmol),反應(yīng)進程通過薄層色譜(TLC)監(jiān)測。反應(yīng)完成后,用鹽酸(HCl)溶液將反應(yīng)混合物的pH調(diào)節(jié)至5至6,隨后進行過濾,并用二氯甲烷(DCM,100mL×3)萃取。合并有機相,用無水硫酸鈉(Na2SO4)干燥,過濾后減壓濃縮,得到3-羥基氮雜環(huán)庚烷-1-甲酸叔丁酯(油狀物,4.8g,收率87%)。產(chǎn)物結(jié)構(gòu)通過1H NMR(400MHz,d6-DMSO)確認:δppm3.95-3.93(m,1H),3.71-3.62(m,2H),3.40(m,1H),3.32-3.28(m,1H),3.03(m,1H),1.88-1.65(m,4H),1.55-1.36(m,11H)。
參考文獻:
[1] Patent: US2017/313683, 2017, A1. Location in patent: Paragraph 1046-1047
[2] Patent: WO2012/80990, 2012, A1. Location in patent: Page/Page column 129-130
[3] Patent: US2012/190678, 2012, A1. Location in patent: Page/Page column 80
[4] Process Biochemistry, 2017, vol. 56, p. 90 - 97
[5] Patent: WO2018/26371, 2018, A1. Location in patent: Paragraph 0174