55 results about "Diethyl azodicarboxylate" patented technology

The invention discloses a method for synthesizing enantiomorphous pure symmetric trans-dialkyl cyclohexylamine, belonging to the field of chemistry. The method comprises the following steps of: carrying out an airtight or reflux reaction on cyclohexene oxide and an aqueous solution of alkylamine for reacting at 80-120 DEG C for 1.5-5h to obtain 2-alkyl-amino cyclohexanol, dropwise adding DEAD (Diethyl Azodicarboxylate) or DIAD (Diisopropyl Azodicarboxylate) to triphenylphosphine, 2-alkyl-amino cyclohexanol and a solvent under an ice bath for reacting for 5-20h at room temperature to obtain N-alkyl-7-azabicyclo[4, 1, 0]heptane, adding a catalyst to the N-alkyl-7-azabicyclo[4, 1, 0]heptane and the aqueous solution of alkylamine at 100-120 DEG C to carry out the airtight or reflux reaction to obtain trans-N,N'-dialkyl-1,2 cyclohexanamine, dissolving the trans-N,N'-dialkyl-1,2 cyclohexanamine in an alcoholic solvent, and adding a tartaric acid type resolving agent with the equivalent weight of 0.5 to the alcoholic solvent to resolve so as to obtain the enantiomorphous pure symmetric trans-dialkyl cyclohexylamine.

The invention provides a preparation method of ketorolac tromethamine. 5-benzoyl-2, 3-dihydro-1H-dilazine-1 and 1-diethyl azodicarboxylate are the starting materials and are prepared into salt by alkaline hydrolysis and acidification when reducers exist, and finally, the salt is prepared into ketorolac tromethamine. The method does not need complicated decarboxylation process, and effectively solves the problems of low purity, poor color and the like caused by the oxidizability of ketorolac. The invention has the advantages of simple operation, high yield and high purity (the total yield in two steps reaches 95% and the purity reaches more than 99.9%); thus, the preparation method is suitable for large-scale commercial process.

The invention relates to a synthetic method and application of a redox induced pH-responsive type methacrylate fluorine-containing monomer. The general formula is shown in the specification, wherein a, b, c and d are respectively independent integers. The synthetic method comprises the following steps: with organic alkali as an acid-binding agent, enabling a methacrylate monomer containing a primary amine end group to react with 2,4-dinitrobenzene sulfonyl chloride in anhydrous tetrahydrofuran so as to obtain a sulfamide monomer; and with diethyl azodicarboxylate and triphenylphosphine as catalysts, enabling the sulfamide monomer to have a Mitsunobu reaction with a fluorine alcohol monomer, separating and purifying, and assembling in an aqueous solution. A strong electron withdrawing group2,4-dinitro-benzsulfamide exists in the structure disclosed by the invention and can rapidly have a nucleophilic substitution reaction with mercapto group so as to produce a secondary amine group, and the secondary amine group is protonized under corresponding pKa, so that redox induced pH response is realized. Development of fluorine-containing small molecules is facilitated, and the developmentneed of a 19FMRI probe is met. The synthetic method disclosed by the invention is simple, and the monomer is stable in quality and high in yield. The structural formula is as shown in the specification.

The present invention proposes a preparation method of edoxaban tosylate intermediate: obtained through the following reaction steps: the specific steps are: step a: under certain temperature conditions, use diformamide-substituted cyclohexylaminoalcohol, triphenyl Phosphine (PPh 3 ), diethyl azodicarboxylate (DEAD) in a solvent, then add N-(tert-butoxycarbonyl) p-nitrobenzenesulfonamide or N-(tert-butoxycarbonyl)-p-toluenesulfonamide to react to obtain hand Compound 2 after sex reversal; step b: remove Boc under strongly acidic conditions to obtain compound 1. The present invention also proposes intermediate compounds in the preparation of edoxaban tosylate intermediates: compounds and compounds. Sodium is beneficial to improve process safety and increase production yield.

The invention belongs to the technical field of functional macromolecules, and in particular relates to a preparation method for synthesizing trans-4-(β-bromovinyl)phenoxy benzyl resin (I). The present invention adopts trans-4-(β- Bromovinyl) phenol and Wang resin were used as raw materials, and trans-4-(β-bromoethylene containing bromoethylene active groups was synthesized at room temperature in tetrahydrofuran, triphenylphosphine, and diethyl azodicarboxylate system. base) phenoxy benzyl resin. The trans-4-(beta-bromovinyl) phenoxy benzyl resin synthesized by this method takes vinyl bromide as a reactive group, and can be used as a starting material for the combinatorial chemical synthesis of many types of compounds for use in medicines, pesticides, Synthesis of physiologically active natural products, liquid crystals, functional materials, etc.