156866-52-3

基本信息
4-甲酰芐基氨基甲酸叔丁酯
(4-甲?;?甲氨基甲酸叔丁酯
(4-甲?;S基)氨基甲酸叔丁酯
4-[(BOC-氨基)甲基]苯甲醛
N-[(4-甲?;交?甲基]氨基甲酸叔丁酯
N-Boc-4-(Aminomethyl)benzaldehyde
tert-butyl 4-formylbenzylcarbamate
TERT-BUTYL N-(4-FORMYLBENZYL)CARBAMATE
4-(N-TERTBUTOXYAMINOMETHYL)BENZALDEHYDE
4-(Aminomethyl)benzaldehyde, N-BOC protected
Tert-butylN-[(4-formylphenyl)methyl]carbamate
(4-formyl-benzyl)-carbamic acid t-butyl ester
(4-Formylbenzyl)carbamic acid tert-butyl ester
tert-Butyl (4-formylbenzyl)carbamate, 4-{[(tert-Bu
物理化學(xué)性質(zhì)
安全數(shù)據(jù)
制備方法

123986-64-1

156866-52-3
以4-(羥甲基)芐基氨基甲酸叔丁酯為原料合成4-甲酰芐基氨基甲酸叔丁酯的一般步驟:將4-(羥甲基)芐基氨基甲酸叔丁酯(2.20g,9.2mmol)溶于二氯甲烷(DCM,100ml)中,加入二氧化錳(MnO2,8.18g,92mmol,10當(dāng)量)。將所得懸浮液在室溫下攪拌3小時。反應(yīng)完成后,將反應(yīng)混合物通過硅藻土過濾,以去除不溶性雜質(zhì)。濾液經(jīng)減壓濃縮,得到4-甲酰芐基氨基甲酸叔丁酯,為白色固體(2.18g,9.2mmol,收率100%)。薄層色譜(TLC)分析顯示Rf = 0.62(展開劑:DCM/乙酸乙酯,9:1)。紅外光譜(IR)顯示特征吸收峰。核磁共振氫譜(1H NMR,300MHz,CDCl3)δ = 10.0(s, 1H, CHO),7.85(d, J = 8.1Hz, 2H, ArCH adjacent to CHO),7.45(d, J = 8.1Hz, 2H, ArCH adjacent to CH2NHBoc),4.99(bs, 1H, NHBoc),4.40(d, J = 5.7Hz, 2H, CH2NHBoc),1.47(s, 9H, C(CH3)3)。核磁共振碳譜(13C NMR,75MHz,CDCl3)δ = 191.9(CHO),155.9(CO),145.9(ArCCH2NHBoc),135.5(ArCCHO),130.1(ArCH adjacent to CHO),127.6(ArCH adjacent to CH2NHBoc),85.1(C(CH3)3),44.3(CH2NHBoc),28.3(C(CH3)3)。高分辨質(zhì)譜(HRMS,ESI+)顯示m/z為258.1101(計算值:C13H19NO3Na [M+Na]+,258.1101;實測值:258.1094)。核磁共振數(shù)據(jù)與文獻(xiàn)報道一致。
參考文獻(xiàn):
[1] Patent: WO2012/95628, 2012, A1. Location in patent: Page/Page column 18-19
[2] Patent: WO2006/117549, 2006, A1. Location in patent: Page/Page column 148
[3] Patent: WO2005/12280, 2005, A1. Location in patent: Page/Page column 53
[4] Patent: WO2006/12135, 2006, A1. Location in patent: Page/Page column 49-51
[5] Patent: US2006/293379, 2006, A1. Location in patent: Page/Page column 63