Urbanczyk-Pearson Lauren M, Meade Thomas J
Department of Chemistry, Department of Biochemistry and Molecular and Cell Biology, Department of Neurobiology and Physiology, Department of Radiology, Northwestern University, Evanston, Illinois 60201, USA.
Nat Protoc. 2008;3(3):341-50. doi: 10.1038/nprot.2007.529. Epub 2008 Feb 14.
The preparation of beta-EgadMe and alpha-EgadMe, magnetic resonance (MR) contrast agents that can be used for in vivo detection of beta-galactosidase, is described. Diastereomerically pure beta-EgadMe can be synthesized by kinetically resolving the starting material as described in Step 1. The total time for the preparation of the racemic mixture of beta-EgadMe is about 8 d, and the total time for an diastereomerically resolved agent is about 9 d. The final metallated agent is stable at room temperature as a solid or in aqueous buffer (pH 5.5-10) indefinitely. Diastereomerically pure alpha-EgadMe can be prepared by beginning the synthesis with enantiomerically pure bromopropionic acid. The total time for the preparation of racemic alpha-EgadMe or diastereomerically pure alpha-EgadMe is about 8 d. The final metallated agent is stable at room temperature as a solid or in aqueous buffer (pH 5.5-10) indefinitely.
本文描述了β-EgadMe和α-EgadMe这两种磁共振（MR）造影剂的制备方法，它们可用于体内检测β-半乳糖苷酶。非对映体纯的β-EgadMe可通过如步骤1所述对起始原料进行动力学拆分来合成。制备β-EgadMe外消旋混合物的总时间约为8天，制备非对映体拆分试剂的总时间约为9天。最终的金属化试剂作为固体或在水性缓冲液（pH 5.5 - 10）中在室温下可无限期稳定保存。非对映体纯的α-EgadMe可通过以对映体纯的溴丙酸开始合成来制备。制备外消旋α-EgadMe或非对映体纯α-EgadMe的总时间约为8天。最终的金属化试剂作为固体或在水性缓冲液（pH 5.5 - 10）中在室温下可无限期稳定保存。
