1986-81-8Relevant articles and documents
Synthetic method for drug intermediate nicotinamide-N-oxide
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Paragraph 0014; 0017-0028, (2018/07/30)
The invention discloses a synthetic method for the drug intermediate nicotinamide-N-oxide. The synthetic method comprises the following steps: adding 3-methylpyridine and a potassium chloride solutioninto a reaction vessel, controlling a stirring speed to be 150-180 rpm, controlling a solution temperature to be 40-45 DEG C, adding a diethyl fumarate solution and a 1,3-propanediamine solution, adding N-chloroacetamide in batches within 30-50 min, and continuing a reaction for 80-100 min; and adding manganese chloride powder, controlling the stirring speed to be 230-250 rpm, continuing the reaction for 3-5 h, adding a sodium sulfate solution, subjecting the obtained solution to layering, separating an oil layer, washing the oil layer with a potassium bromide solution for 30-50 min, then washing the oil layer with a chloroprene solution for 20-40 min, carrying out recrystallization in a glycol monomethyl ether solution and then carrying out dehydration with a dehydrating agent so as to obtain the finished nicotinamide-N-oxide.
Renewable waste rice husk grafted oxo-vanadium catalyst for oxidation of tertiary amines to N-oxides
Panwar, Vineeta,Bansal, Ankushi,Ray, Siddharth S.,Jain, Suman L.
, p. 71550 - 71556 (2016/08/05)
Low cost renewable waste rice husks (RH) have been used as a support for grafting of an oxo-vanadium Schiff base via covalent attachment for the oxidation of tertiary amines to N-oxide. The synthesis of the desired RH grafted oxo-vanadium complex involves prior functionalization of the RH support with amino-propyltrimethoxysilane (APTMS) followed by its reaction with salicylaldehyde to get an RH-functionalized Schiff base which subsequently reacted with vanadyl sulphate to get the targeted oxo-vanadium catalyst. The synthesized catalyst was found to be an efficient heterogeneous catalyst and afforded an excellent yield of corresponding N-oxides via oxidation of tertiary amines with hydrogen peroxide as an oxidant. Furthermore, the synthesized catalyst was found to be quite stable and showed consistent activity for five runs without any loss in activity.
Trichloroacetonitrile-hydrogen peroxide: A simple and efficient system for the selective oxidation of tertiary and secondary amines
Nikbakht, Fatemeh,Heydari, Akbar
, p. 2513 - 2516 (2014/05/06)
A variety of tertiary and secondary amines were efficiently oxidized to their corresponding N-oxides and nitrones, respectively, using the trichloroacetonitrile-hydrogen peroxide system. The in situ generated trichloromethylperoxyimidic acid is the active reagent for the oxidation processes.