3430-13-5Relevant articles and documents
Synthesis of C-14 and C-13, H-2-labeled IKK inhibitor: [14C] and [13C4,D3]-N-(6-chloro-7-methoxy-9H-pyrido3,4- blindol-8-yl)-2-methyl-3-pyridinecarboxamide
Li, Yuexian,Plesescu, Mihaela,Prakash, Shimoga R.
, p. 789 - 799 (2006)
[14C]-N-(6-Chloro-7-methoxy-9H-pyrido [3,4-b]indol-8-yl)-2- methyl-3-pyridinecarboxamide (5B), an IKK inhibitor, was synthesized from [ 14C]-barium carbonate in two steps in an overall radiochemical yield of 41%. The intermediate, [carboxyl-14C]-2-methylnicotinic acid, was prepared by the lithiation and carbonation of 3-bromo-2-methylpyridine. [ 13C4,D3]-N-(6-chloro-7-methoxy-9H-pyrido[3,4-b] indol-8-yl)-2-methyl-3-pyridinecarboxamide (5C) was synthesized from [1,2,3,4-13C4]-ethyl acetoacetate and [D 4]-methanol in six steps in an overall yield of 2%. [ l3C4]-2-methylnicotic acid, was prepared by condensation of [13C4]-ethyl 3-aminocrotonate and acrolein, followed by hydrolysis with lithium hydroxide. Copyright
A 2 - bromo -4 - pyridylaldehyde preparation method (by machine translation)
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Paragraph 0017; 0019; 0020; 0024, (2019/05/28)
The invention belongs to the field of organic synthesis, in particular relates to a 2 - bromo - 4 - pyridylaldehyde preparation method, comprises the following steps: (1) 2 - bromo - 4 - methyl pyridine preparation: will be hydrobromic arranged in four bottle, added under mixing 2 - amino - 4 - methylpyridine, to be 2 - amino - 4 - methyl pyridine completely after dissolving, cooling to - 20 °C, slow [...], dropping process control temperature is - 20 °C - - 15 °C; dropped stirring for 90 - 120 min, then dropping sodium nitrite solution, after adding, the temperature to 20 °C, stirring 45 - 60 min and then cooling to - 20 °C - - 25 °C, sodium hydroxide solution, dropping process control temperature is lower than - 15 °C - - 10 °C; after adding, the temperature is raised to 20 °C and stirring 1 h, extraction, the combined organic phase, washing, drying, concentration; (2) 2 - bromo - 4 - pyridylaldehyde preparation. The beneficial effect of the invention is: mild reaction conditions, is easy to operate, after treatment is simple, and easy to enlarge production, is extremely suitable for industrial production; high yield, low prices of raw materials, the production cost is low. (by machine translation)
Complexes of 4- and 5-bromo derivatives of 2-(hydroxymethyl)pyridine with copper(II) and cobalt(II) salts. Synthesis and X-ray crystal structures
Hubrich, Michael,Peukert, Max,Seichter, Wilhelm,Weber, Edwin
body text, p. 1854 - 1862 (2010/07/04)
Four copper(II) complexes (1-4) and a cobalt(II) complex (5) derived from 4-bromo-2-(hydroxymethyl)pyridine (L1) or 5-bromo-2-hydroxymethyl)pyridine (L2) with Cu(NO3)2·3H2O, CuCl2·2H2O and CoCl2·6H2O have been synthesized and their respective crystal structures studied. They show specific influences owing to the different kind of metal cations and counter anions, the hydration as well as the different position of the bromine substitution on both the coordination of the complex unit and the network structure of the crystal lattice. The Cu(II) complexes of L1 are five-coordinate [Cu(L1)2NO3]NO3·H2O (1) and [Cu(L1)2Cl]Cl·H2O (2) species with distorted quadratic pyramidal and trigonal bipyramidal coordination geometries of the N2O3 and N2O2Cl donor atoms around the Cu(II), respectively. The Cu(II) complexes of L2 are six-coordinate [Cu(L2)2(NO3)2] (3) and [Cu(L2)2Cl(H2O)]Cl·H2O (4) species with distorted octahedral coordination geometries of the N4O2 and N2O3Cl donor atoms. A distorted octahedral coordination geometry of the N2O2Cl2 donor atoms is also found in the complex unit [Co(L2)2Cl2] of the Co(II) complex 5 but showing the oxygen atoms of the chelating ligand as well as the chloride ions in a cis-position. Depending on the complex, water molecules and chloride anions are shown to act as stabilizing components of the crystal structure. The comparative structural investigation includes also known structures of the bromine-free ligand analogue 2-(hydroxymethyl)pyridine, illustrating the basic implication of the bromine substitution, mostly perceptible in the different modes of crystal packing.