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33results about How to "Increased weight yield" patented technology

Method for preparing 17alpha-hydroxyprogesteron

The invention relates to a method for preparing 17alpha-hydroxyprogesterone. The17alpha-hydroxyprogesterone is prepared by taking 17beta- cyano-5-androstene-17-ol-3,3-diethylene ketal (referred as an intermediate II) as a raw material and dimethylzinc or methylzinc chloride as a reagent; the content of the 17alpha-hydroxyprogesterone by HPLC is above 99.5% and the weight yield is 83-87%. The method comprises the following steps of dissolving the intermediate II in an organic solvent, adding lithium chloride as a catalyst, stirring, raising the temperature to 40-80 DEG C, dropwise adding a toluene solution of dimethylzinc or methylzinc chloride of which the concentration is 2M, and continuing to complete the reaction; and then adding an ammonium chloride solution of which the concentration is 25% to destruct an organic zinc reagent, separating the aqueous layer out and extracting, merging the organic layer and the extract and concentrating the solvent to near dryness, and then adding lower alcohol, stirring, raising the temperature to 40-60 DEG C, adding the acid of which the concentration is 2M, hydrolyzing, adjusting the pH value with a weak base after the reaction is completed, evaporating 90% of the solvent out, adding tap water, cooling and crystallizing to obtain a crude 17alpha-hydroxyprogesterone product; and then carrying out reflux decolorizing on the crude product with activated carbon by virtue of alcohol, and refining to obtain the commercial grade 17alpha-hydroxyprogesterone. The 17alpha-hydroxyprogesterone produced by the method disclosed by the invention has the advantages of good purity and high yield and is economic and environment-friendly, and the solvent can be recycled.
Owner:HUNAN KEREY BIOTECH

Method for preparing mixture of ortho vanillin and vanillin

The invention relates to a method for preparing a mixture of ortho vanillin and vanillin, which is applied to the field of medicine synthesis. The method comprises the following steps of: taking guaiacol and chloroform as raw materials; taking carbinol as a medium; reacting under the condition that sodium hydroxide aqueous solution is added; and utilizing acid to adjust the pH value of the obtained products to be at acid level, thereby obtaining the mixture of ortho vanillin and vanillin, wherein the weight ratio of guaiacol to chloroform to carbinol to sodium hydroxide is (40-60): (200-280): (20-45): (50-80); the concentration of the sodium hydroxide aqueous solution is 40-50%; the reaction temperature in the preparing method is 55 DEG C; the holding time is 4 hours; and the pH value is 5-6. The method further comprises the step of steaming carbinol from the mixture and distilling and removing dregs; the process of steaming carbinol comprises the following steps of: pumping and filtering the mixture, carrying out distilling under reduced pressure by a water pump at 40 DEG C and drying the carbinol, thereby obtaining an oily matter; and the oily matter is subjected to distilling under reduced pressure for 30 minutes at 60 DEG C, thereby obtaining oily liquid. According to the method provided by the invention, the yield of total weight is high and the proportion of the ortho vanillin is increased.
Owner:NORTHEAST PHARMA GRP

Oxidation catalyst as well as preparation method and application thereof

The invention discloses an oxidation catalyst and a preparation method and application thereof, wherein the oxidation catalyst comprises a first vanadium-molybdenum catalyst and / or a second vanadium-molybdenum catalyst, the first vanadium-molybdenum catalyst and / or the second vanadium-molybdenum catalyst independently contain vanadium, molybdenum, nickel and an auxiliary agent, and wherein, the average oxidation state of vanadium in the first vanadium-molybdenum catalyst is lower than the average oxidation state of vanadium in the second vanadium-molybdenum catalyst. In the process of preparing the catalytic active substance precursor, the oxidation state of the main metal vanadium in the active substance precursor is modulated by using an oxidation-reduction reaction, and the main metal vanadium is coupled with different types of metal additives. When the catalyst is applied to a reaction for oxidative synthesis of maleic anhydride, under the condition that the benzene concentration is 40-65 g / Nm3, the benzene conversion rate reaches more than 98%, and the weight yield of maleic anhydride reaches 94-99%. Under the same operation conditions, the conversion rate of benzene can be increased by 3.6% at most, and the weight yield of maleic anhydride can be increased by 4.4% at most.
Owner:CHINA PETROLEUM & CHEM CORP +1

Method for preparing sodium 7-methoxy-7-chloracetylamino-3-methyltetrazole sulfidomethyl cephalosporanic acid

InactiveCN101423523BCompletely precipitatedMild reaction conditionsOrganic chemistrySolventEthyl Chloride
The invention discloses a preparation method for 7-methoxy-7-chloracetyl amido-3-methyl tetrazole s-methyl sodium cephalosporanic acid. The method comprises the following steps: adding 7-methoxy-7-chloracetyl amido-3-methyl tetrazole s-methyl cephalosporanic acid benzyl ester and trifluoroacetic acid in turn into the phenolic compound solvent for reaction; adding ethyl acetate into the reaction liquor when the reaction residue is less than 1 percent; adjusting the pH value of the reaction liquor to form an organic phase and a water phase; taking the water phase and adding ethyl acetate into the water phase; after even mixing, regulating the pH value, splitting phases through standing, collecting the organic phase after extraction, and then carrying out concentration and drying; adding theorganic phase into ethanol isopropyl alcohol mixed liquor; stirring to dissolve the organic phase, adding sodium iso-octoate and isopropyl alcohol mixed liquor into the mixed solution for reaction; cooling, filtrating and drying the product after the reaction to obtain the finished product. The method saves the preparation process of adopting an alchlor catalyst; and simultaneously trifluoroacetic acid is added into the solvent of o-cresol, m-cresol or p-cresol for benzyl ester removing hydrolysis, thereby not only shortening the technical flow and simplifying the operation, but also improving the yield to 75 to 80 percent.
Owner:河北九派制药股份有限公司
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