http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-102659637-B

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http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C275-64
filingDate 2012-05-21-04:00^^<http://www.w3.org/2001/XMLSchema#date>
grantDate 2014-05-14-04:00^^<http://www.w3.org/2001/XMLSchema#date>
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publicationDate 2014-05-14-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-102659637-B
titleOfInvention Method for preparing dihydroxyurea
abstract The invention relates to a novel method for preparing dihydroxyurea and belongs to the field of organic synthesis. The dihydroxyurea belongs to a novel salt-free reducing agent which is used for spent fuel post treatment and has good application prospects. The novel method is mainly characterized in that under the anhydrous conditions, solid phosgene and hydroxylamine are used for synthesizing the dihydroxyurea. Concretely, hydroxylamine and potassium acetate are firstly placed into a three-opening flask, are placed into an ice salt bath and are stirred into emulsion. In addition, the solid phosgene is dissolved into 1, 4-dioxane, the mixed liquid is placed into a constant-pressure liquid dripping funnel, when the temperature is below 0 DEG C, the solid phosgene mixing liquid is dripped into the emulsion at the controlled speed, and the temperature is maintained at 0 to 5 DEG C. The reaction is continuously carried out for 2 hours after the dripping completion, and then, the pH of the solution is regulated to 2 to 3 through concentrated hydrochloric acid. Solid materials are removed through filtering, solvents are removed through rotary evaporation on filter liquid, and solid is obtained. A proper amount of tetrahydrofuran is used for extracting the dihydroxyurea in the solid, the solvents are removed through the rotary evaporation, coarse dihydroxyurea is obtained, ethanol is used for recrystallization, and the pure dihydroxyurea is obtained. Through the detection and characterization on products by various methods, the product purity is 95 percent, and the yield is 57 percent.
priorityDate 2012-05-21-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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