Shetty H U, Nelson W L
J Pharm Sci. 1985 Sep;74(9):968-71. doi: 10.1002/jps.2600740912.
Cyanide anion was used to attempt to trap possible imine intermediates in the oxidative N-dealkylation of propranolol (1). Reaction of 3-(1-naphthoxy)-1-amino-2-propanol (desisopropylpropranolol, 2) with acetone provided this expected intermediate in an approximately 7:1 ratio of oxazolidine 6 to imine 5, as determined by 1H NMR. The mixture when treated with sodium cyanide gave the expected alpha-aminonitrile 7. Microsomal oxidation of propranolol in the presence of sodium cyanide gave two cyanide-containing adducts as shown by GC-MS (12a and 12b). Using specifically deuterated propranolols (8, 9, 10, and 11) as substrates showed both of these cyanide-containing adducts to have lost the N-isopropyl group. Compounds 12a and 12b were shown to be diastereomeric alpha-aminonitriles arising from the reaction of 2 with propionaldehyde, a contaminant from the ether used for extraction, and cyanide anion. Authentic 7, stable to derivatization and GC-MS conditions, rapidly decomposed under the conditions of the metabolic experiments.
使用氰根阴离子尝试捕获普萘洛尔(1)氧化N-脱烷基化过程中可能的亚胺中间体。3-(1-萘氧基)-1-氨基-2-丙醇(去异丙基普萘洛尔,2)与丙酮反应,通过1H NMR测定,以大约7:1的恶唑烷6与亚胺5的比例得到了这种预期的中间体。用氰化钠处理该混合物得到了预期的α-氨基腈7。在氰化钠存在下,普萘洛尔的微粒体氧化通过GC-MS显示得到了两种含氰加合物(12a和12b)。使用特定氘代的普萘洛尔(8、9、10和11)作为底物表明,这两种含氰加合物都失去了N-异丙基基团。化合物12a和12b被证明是由2与丙醛(用于萃取的乙醚中的一种污染物)和氰根阴离子反应产生的非对映体α-氨基腈。纯正的7对衍生化和GC-MS条件稳定,但在代谢实验条件下迅速分解。