Bacsa Bernadett, Kappe C Oliver
Christian Doppler Laboratory for Microwave Chemistry (CDLMC) and Institute of Chemistry, Karl-Franzens-University Graz, Graz, Austria.
Nat Protoc. 2007;2(9):2222-7. doi: 10.1038/nprot.2007.300.
A rapid and efficient microwave-assisted solid-phase synthesis method for the preparation of a nonapeptide using conventional Fmoc/Bu(t) orthogonal protection strategy is described. In this protocol, the coupling steps are performed within 5 min at 60 degrees C and the Fmoc-deprotection steps are completed within 3 min at 60 degrees C using a dedicated single-mode microwave peptide synthesizer utilizing temperature-controlled conditions. It is demonstrated that the model nonapeptide (containing the calmodulin-binding octapeptide sequence) is synthesized in a shorter time (approximately 3.5 h) and with high purity (>95%) under microwave irradiation conditions in comparison with a reference peptide that is obtained by standard methods at room temperature (within 11 h).
描述了一种使用传统的Fmoc/Bu(t)正交保护策略快速高效地微波辅助固相合成九肽的方法。在此方案中,使用温度控制条件的专用单模微波肽合成仪,偶联步骤在60℃下5分钟内完成,Fmoc脱保护步骤在60℃下3分钟内完成。结果表明,与在室温下通过标准方法获得的参考肽(11小时内)相比,模型九肽(包含钙调蛋白结合八肽序列)在微波辐射条件下合成时间更短(约3.5小时)且纯度更高(>95%)。