Department of Chemistry, Washington State University, PO BOX 644630, Pullman, WA 99164-4630, USA.
Chemistry. 2010 Jul 19;16(27):8096-107. doi: 10.1002/chem.201000185.
The mechanism of N-dealkylation mediated by cytochrome P450 (P450) has long been studied and argued as either a single electron transfer (SET) or a hydrogen atom transfer (HAT) from the amine to the oxidant of the P450, the reputed iron-oxene. In our study, tertiary anilinic N-oxides were used as oxygen surrogates to directly generate a P450-mediated oxidant that is capable of N-dealkylating the dimethylaniline derived from oxygen donation. These surrogates were employed to probe the generated reactive oxygen species and the subsequent mechanism of N-dealkylation to distinguish between the HAT and SET mechanisms. In addition to the expected N-demethylation of the product aniline, 2,3,4,5,6-pentafluoro-N,N-dimethylaniline N-oxide (PFDMAO) was found to be capable of N-dealkylating both N,N-dimethylaniline (DMA) and N-cyclopropyl-N-methylaniline (CPMA). Rate comparisons of the N-demethylation of DMA supported by PFDMAO show a 27-fold faster rate than when supported by N,N-dimethylaniline N-oxide (DMAO). Whereas intermolecular kinetic isotope effects were masked, intramolecular measurements showed values reflective of those seen previously in DMAO- and the native NADPH/O(2)-supported systems (2.33 and 2.8 for the N-demethylation of PFDMA and DMA from the PFDMAO system, respectively). PFDMAO-supported N-dealkylation of CPMA led to the ring-intact product N-cyclopropylaniline (CPA), similar to that seen with the native system. The formation of CPA argues against a SET mechanism in favor of a P450-like HAT mechanism. We suggest that the similarity of KIEs, in addition to the formation of the ring-intact CPA, argues for a similar mechanism of Compound I (Cpd I) formation followed by HAT for N-dealkylation by the native and N-oxide-supported systems and demonstrate the ability of the N-oxide-generated oxidant to act as an accurate mimic of the native P450 oxidant.
细胞色素 P450(P450)介导的 N-脱烷基化的机制长期以来一直被研究和争论,认为是从胺到 P450 的氧化剂(所谓的铁氧体)的单个电子转移(SET)或氢原子转移(HAT)。在我们的研究中,叔胺 N-氧化物被用作氧代,以直接生成 P450 介导的氧化剂,该氧化剂能够对二甲氨基苯衍生的氧供体进行 N-脱烷基化。这些替代物被用来探测生成的活性氧物种和随后的 N-脱烷基化机制,以区分 HAT 和 SET 机制。除了预期的产物苯胺的 N-脱甲基化外,还发现 2,3,4,5,6-五氟-N,N-二甲基苯胺 N-氧化物(PFDMAO)能够对 N,N-二甲基苯胺(DMA)和 N-环丙基-N-甲基苯胺(CPMA)进行 N-脱烷基化。由 PFDMAO 支持的 DMA 的 N-脱甲基化的速率比较表明,其速率比由 N,N-二甲基苯胺 N-氧化物(DMAO)支持时快 27 倍。尽管分子间动力学同位素效应被掩盖,但分子内测量显示的值反映了先前在 DMAO 和天然 NADPH/O2 支持系统中看到的值(分别为 PFDMAO 系统中 PFDMA 和 DMA 的 N-脱甲基化的 2.33 和 2.8)。PFDMAO 支持的 CPMA 的 N-脱烷基化导致环完整产物 N-环丙基苯胺(CPA),类似于天然系统。CPA 的形成反对 SET 机制,有利于 P450 样 HAT 机制。我们认为,除了形成环完整的 CPA 外,KIE 的相似性也支持了天然和 N-氧化物支持的系统中 Cpd I 形成后的类似 HAT 机制,并证明了 N-氧化物生成的氧化剂能够充当天然 P450 氧化剂的准确模拟物。