Description machine translated from Chinese One kind of the preparation craft of veratric acid Area of technology This

invention specifically involves one kind of veratric acid the preparation craft. Background technology The veratric acid may from the Chinese globeflower (Trollius chi-nenisi Baill.), checkerboard is (Zygadenus) veratrum (Veratrum) and reed stem Lilium (Schoeno-caulon offricinale) in plant's seed withdraws to obtain, mainly serves as the chemical reagent. The veratric acid is one kind of commonly used chemical synthesis intermediate, widely applies in industry, medicine, agricultural chemicals and other domains, is synthesizes medicine muriatic acid Arab League [fu] the azole [qin] and other chemical compound key intermediates. Shortcoming that past the preparation craft of veratric acid had: (1) mainly takes the black false hellebore mellowly as raw material, after oxidized production veratric acid. This method's major object is The raw material is more expensive, and responded that often has indefinite quantity the production of by-product veratraldehyde, the yield generally is not very high. (2) mainly takes the veratraldehyde as outset raw material, takes the methanol as the resolver, has the disproportionation response production salt the aldehyde and alkali, then acidifies, this method cost is high, production rate is low. Invention content Goal of this invention is to provide one kind of cost is low, purity is high, the preparation craft of yield high veratric acid. For the technical program that to achieve the above goal invention uses is: One kind of the preparation craft of veratric acid, including the following step: (1) under the room temperature adds the 300-800ml water and 60g veratraldehyde in the reflection vessel, Heats up 40.deg.C, stirs melts to veratraldehyde completely; Then joins 30% liquid caustic soda 50-90ml, full stirring, in 40.deg.C starts to add by drops the 180ml hydrogen peroxide solution slowly, 3-5 hours add, the control temperature is 30-35.deg.C; (2) after the hydrogen peroxide solution adds, full stirring, elevates temperature again 55.deg.C, heat preservation; (3) elevates temperature 60.deg.C, after heat preservation 3h, the sample surveys; (4) waits result that the sample surveys to include veratric acid over 99.2%, veratraldehyde content Below 0.5%, decreases temperature to below 25.deg.C, the Canadian 300ml water, adjusts PH=2 with 30% muriatic acids slowly; (5) filters, washes, drains and dry the veratric acid. Stated the step (5), the product after filtration with the room temperature clear water washed PH=5-6, drained latter 80.deg.C dry. In this invention, mainly takes veratraldehyde as the main raw material, takes the water as the resolver, with the alkali salifying, with the hydrogen peroxide solution oxidation, the acidified system results in the veratric acid, skims does with the organic solvent for the method of resolver, the material cost greatly reduces, greatly raised the production efficiency, and achieves in the examination goal content over 95%, the liquid phase content achieves over 99.5%. The product outward appearance assumes the white powder. Implements the way specifically Following implementation example for explaining this invention, but does not need to limit this invention the scope. Implementation example 1: Under the room temperature in the 1000ml four flasks adds the 300-800ml water, the 60g veratraldehyde heats up 40.deg.C, stirs to melt for 10 minutes to the veratraldehyde completely. Then joins 30% liquid caustic soda 50-90ml, stirs for 15 minutes. When 40.deg.C starts to add by drops the 180ml hydrogen peroxide solution slowly, the control temperature 30-35.deg.C, instillment the temperature will have the rise, 3-5 hours add. After the hydrogen peroxide solution adds, stirs for 30 minutes to elevate temperature again 55.deg.C, heat preservation 2h. Then after elevating temperature to 60.deg.C heat preservation 3h, the sample surveys; Testing quantity's result includes veratric acid over 99.2%, when veratraldehyde content below 0.5%, decreases temperature to below 25.deg.C, with the 300ml water, adjusts PH=2 with 30% muriatic acids slowly, makes about 24h. The filtration, the press cake washes PH=5-6 with room temperature clear water, drains latter 80.deg.C dry, results in the dried goods approximately 62 g, the outward appearance is the white, content about 99.2%. Test: The product analyzes with [Daojin] highly effective liquid chromatograph, analyzes the condition are as follows, flowing for methanol and water intermixture, methanol: Water =60: 40th, columnar order: C18 250x4.6x5 .micro.m, wave length: 230nm, speed of flow: 1ml/min. The name takes the 0.01g dried goods to dilute with flowing to the 10ml measuring flask, the specimen handling 10.micro.l. The results analysis content achieves >=99.50%

ODES (Trollius chi-nenisi Baill.)(Zygadenus)(Veratrum)(Schoenocaulon offricinale) 1300-800ml60g 4030%50-90ml40180ml 3-530-35 255 3603h 499.2% 0.5%25300ml30%PH=2 5 5PH=5-680 95%99.5% 1 1000ml300-800ml 60g401030%50-90ml15 40180ml30-35,,3-5 30552h603h99.2% 0.5%25300ml30%PH=22-4h PH=5-680 62 g99.2% =60:40 C18 2504.65m230nm1ml/min0.01g 10ml10l99.50