Preparation method of 2-hydroxypyridine-N-oxide

A hydroxypyridine and oxide technology, which is applied in the field of preparation of compound 2-hydroxypyridine-N-oxide, can solve the problems of complex catalyst preparation process, high safety risk factor, high catalyst price and the like, and achieves low cost and industrial convenience. Production, the effect of less organic waste liquid

A hydroxypyridine and oxide technology, which is applied in the field of preparation of compound 2-hydroxypyridine-N-oxide, can solve the problems of complex catalyst preparation process, high safety risk factor, high catalyst price and the like, and achieves low cost and industrial convenience. Production, the effect of less organic waste liquid

CN102001995AInactive Publication Date: 2011-04-06湖南欧亚药业有限公司
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  • Preparation method of 2-hydroxypyridine-N-oxide
  • Preparation method of 2-hydroxypyridine-N-oxide
  • Preparation method of 2-hydroxypyridine-N-oxide

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[0019] In order to make the technical means, creative features, work flow, and use methods of the present invention achieve the purpose and effect easily understood, the present invention will be further described below in conjunction with specific illustrations.

[0020]

[0021] Add 30 kg of 2-chloropyridine, 200 kg of tap water, 1.5 kg of sodium tungstate, and 2 kg of concentrated sulfuric acid into a 500L reactor, and stir until it dissolves; raise the temperature to 55°C, and slowly add 100 kg of 30% hydrogen peroxide dropwise; the addition is complete Continue reaction at this temperature for 48 hours afterward, HPLC test raw material conversion rate is 84%, be cooled to room temperature, add 12.3 kilograms of liquid caustic soda and adjust to neutrality, add 50 kilograms of toluene, extract unreacted raw material (this layer can be concentrated and reclaimed toluene and raw materials); adding 20 kg of sodium hydroxide to the water layer, reflux reaction for 8 hours, H...

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Abstract

The invention discloses a preparation method of an important intermediate: 2-hydroxypyridine-N-oxide with the CAS Number of 13161-30-3. The invention reports a new synthetic route applicable to industrial production, which comprises the following steps: under catalysis of a catalyst generated in-situ, oxidizing 2-chloropyridine with hydrogen peroxide (30%) to generate an N-oxide, and then hydrolyzing under an alkaline condition to directly generate the target product. The preparation method greatly improves the yield, realizes one-pot reaction, greatly reduces generation of organic waste liquor and realizes environmental protection.

Description

technical field [0001] The invention relates to a synthesis method of a compound, in particular to a preparation method of the compound 2-hydroxypyridine-N-oxide. Background technique [0002] 2-Hydroxypyridine-N-oxide is an important compound. Recent studies have found that this compound has a special role in preventing and controlling wood degradation due to white-rot fungi; it is also a new type of effective Iron chelating agent; and the complex formed by this compound and vanadium also plays an important role in biochemistry. [0003] The synthetic routes of 2-hydroxypyridine-N-oxide are mainly following three routes. [0004] Route 1 [M.Ramakrishna Prasad et al, Chem.Commun.2000, 17:1577-1578]: [0005] [0006] Route 2 [Lohkov, R.E.etal, Chem.Heterocycl.Compd.(Engl.Transl.) 1980, 16:264-271] [0007] [0008] Route 3【Saul Wolfe et al.Chemistry-A European Journal.1998, 4:886-902】 [0009] [0010] Wherein the catalyst preparation process that route one adop...

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Application Information

Patent Timeline
06 Apr 2011
Publication
CN102001995A
IPC
C07D213/89
Inventors
林开朝