4-氨基-2-甲基-1-丁醇的合成

设计并合成了一种重要药物中间体4-氨基-2-甲基-1-丁醇。以异丁烯醇、乙酰氯为初始原料，经酯化反应、氢甲酰化反应、胺化还原反应和水解反应制得目标产物。经优化后的反应条件如下:氢甲酰化反应中膦配体/铑催化剂的摩尔比为4∶1，反应温度为120 ℃，合成气（CO/H₂）压力为3 MPa，反应得到中间体醛；胺化还原反应中兰尼镍/底物醛的质量比为1∶20，H₂压力为0.9 MPa，反应得到中间体胺。最后，通过核磁共振氢谱对产物进行了表征，确认目标产物为4-氨基-2-甲基-1-丁醇。产物的总收率为62%。该合成路线原料易得，条件温和，流程简便，有实现工业化生产的价值。

Synthesis of 4-Amino-2-Methyl-1-Butanol

4-Amino-2-methyl-1-butanol， an essential intermediate for pharmacy and chemical engineering， was designed and synthesized via methallyl alcohol and acetyl chloride as the starting materials through?esterification， hydroformylation， amination， reduction and hydrolysis. After optimization， the most favorable reaction conditions were as follow: 4∶1 as the mole ratio of phosphine ligand/rhodium catalyst， 120 ℃ as the reaction temperature， 3 MPa as the pressure of syngas （CO/H₂） in hydroformylation for the intermediate containing aldehyde group； and 5% as the mass ratio of Raney Ni/substrate with aldehyde group， 0.9 MPa as the pressure of H₂ in amination and reduction for the intermediate containing amino group. The product was finally confirmed as the target with the 1H NMR characterization with the yield of 62% in term of the starting material isobutenol. The synthesis route is uncomplicated with accessible raw material， and can carried out under mild conditions， which is valuable for industrialization.