9 results about "Diazomethane" patented technology

This invention provides a gas-liquid separator for separating diazonium methane from a diazonium methane mixture. The separator comprises an upper cylinder, a middle cylinder, and a lower cylinder connected sequentially from top to bottom. The upper cylinder has a gas outlet at its top center, surrounded by gas moisture detection ports, diazonium methane content detection ports, gas temperature detection ports, and an explosion vent. A pressure detection port is located on the side. The middle cylinder has a refrigerant inlet and a refrigerant outlet at its upper part, and a refrigerant coil is installed inside the middle cylinder. The refrigerant coil inlet is connected to the refrigerant outlet, and the refrigerant coil outlet is connected to the refrigerant outlet. The lower cylinder has a liquid level-above gas inlet and a liquid level-below gas inlet at its upper part. The liquid level-above gas inlet is connected to a gas distributor above the liquid level via a pipe, and the liquid level-below gas inlet is connected to a gas distributor below the liquid level via a pipe. A feed inlet is located on the middle side wall of the lower cylinder. This gas-liquid separator offers high gas-liquid separation efficiency, is explosion-proof, and can be used for continuous automated production.

The invention discloses a continuous preparation method for carrying out cyclopropanation reaction by using a microreactor. According to the method, a three-stage series bottom splashing microreactor system is adopted, and efficient and safe cyclopropanation reaction is realized through gradient catalysis design and accurate temperature control. A reaction system comprises olefin, a diazomethane precursor, alkali liquor and a solvent, wherein a catalyst adopts a gradient distribution design of SBA-15 and CeO2 loaded monatomic palladium. And the three-stage series bottom splashing microreactors are respectively controlled at different temperatures. The process is simple, high conversion rate and high safety are realized, and the cost is reduced.

The invention discloses a gas chromatography method for detecting the content of trioctyl phosphate products and impurities, and belongs to the technical field of organic chemical detection. The core of the method is that (trimethylsilyl) diazomethane (TMSCH2N2) is adopted as a derivatization reagent, and dioctyl phosphate (P204) in a sample is subjected to rapid and safe derivatization at room temperature; an optimized dichloromethane-hexane mixed solvent system is adopted for dilution, so that the solubility is remarkably improved, and the toxicity is reduced; a first-order heating rapid screening method (17min) is suitable for industrial quality control, a multi-order heating accurate quantification method (29min) is suitable for small-scale test process research and development, and trioctyl phosphate (TOP), P204, isooctyl alcohol, isooctyl ether and chloro-isooctane can be accurately quantified at the same time. The method solves the problems of high toxicity, low efficiency, narrow detection range, single mode and the like in the prior art, and has the remarkable advantages of safety, high efficiency, accuracy, environmental protection and wide adaptability.

The invention relates to a mono-boratriazole compound as well as a synthesis method and application thereof, positive ion boron-nitrogen alkyne and (trimethylsilyl) diazomethane are subjected to cycloaddition reaction, trimethylsilyl is migrated from carbon atoms to nitrogen atoms to form a positive ion mono-boratriazole framework, trimethylsilyl and counter ions are further removed by using alkali, and the mono-boratriazole compound is obtained. The mono-boratriazole compound is obtained. The mono-boratriazole compound disclosed by the invention has a wide application prospect in the fields of metal coordination reaction, reverse cyclization ring-opening reaction and preparation of unsaturated boron compounds.

The invention discloses a method for identifying unknown organic phosphodiesters in an environment based on a diazomethane derivatization technology. The method comprises the following steps: S1, establishing an OPDEs suspicious database; s2, carrying out methyl derivatization on the OPDEs to be detected; s3, carrying out suspicious screening on the OPDEs; s4, determining characteristic fragments of the derivatization OPDEs; and S5, carrying out non-targeted screening on the OPDEs. According to the suspicious-non-targeted comprehensive screening method for the unknown OPDEs in the environmental sample, the limitation that an OPDEs analysis method in the environment can only recognize known types of OPDEs can be solved, and comprehensive recognition of the unknown OPDEs in the environmental sample can be achieved.

The application discloses a viscosity reducer for exploitation of deep low-permeability heavy oil reservoirs and a preparation method and application thereof. The preparation method comprises the following steps: (1) under the conditions of existence of a solvent and a catalyst and heating, 4-halogenophthalic anhydride and glycol compounds are subjected to nucleophilic addition reaction under the atmosphere of nitrogen or inert gas to obtain a mixed solution containing intermediate A; (2) diazomethane is introduced into the mixed solution containing intermediate A, and diazomethane and intermediate A are subjected to nucleophilic transfer reaction to obtain a mixed solution containing intermediate B; (3) polyethylene glycol or dimethylaluminum is added into the mixed solution containing intermediate B, and after stirring, sodium sulfite is added, and under the condition of heating, intermediate B and sodium sulfite are subjected to sulfonation reaction of nucleophilic displacement, and after reaction, the viscosity reducer is obtained through post-treatment. The application further discloses application of the viscosity reducer as a displacement flow-increasing viscosity reducer in exploitation of deep low-permeability heavy oil reservoirs.

The application belongs to the technical field of organic synthesis, and particularly relates to an asymmetric total synthesis method of catharanthine. Commercially available oxazolidinone 1 is used as a starting material, and is condensed with bromoacrylic acid to obtain compound 2. Then, asymmetric DA reaction of compound 2 and compound 3 occurs under the catalysis of scandium triflate to obtain compound 4. Compound 4 is hydrolyzed into a carboxylic acid under the condition of lithium hydroxide and hydrogen peroxide, and is treated by trimethylsilane diazomethane to obtain compound 6. Compound 6 is selectively reacted with sodium methoxide, and after the protective group is removed by treatment of iodo-trimethylsilane, compound 6 is condensed with an acid to obtain compound 9. Compound 9 is subjected to radical annulation under the catalysis of a photocatalyst Ir(ppy)3 to obtain compound 10. Finally, selective reduction of the amide obtains natural product (+) - catharanthine. The asymmetric total synthesis route of the application has a total step of 8 or 9, and a total yield of 17.8% - 23.5%, which is shorter than that of the prior art, and the total yield is significantly improved.

The invention belongs to the field of synthetic chemistry and biological medicine, and particularly relates to a difluoromethyl modified chiral diamine derivative as well as a synthetic method and application thereof. The difluoromethyl modified chiral diamine derivative is obtained by taking p-toluenesulfonyl difluoromethyl diazomethane, aromatic amine, organic aldehyde and electron-rich aromatic hydrocarbon as raw materials and taking chiral phosphoric acid as a chiral inducer and an organic reagent as a solvent through a one-step reaction under the catalysis of transition metal. According to the difluoromethyl modified chiral diamine derivative and the synthesis method, the raw materials are cheap and easy to obtain, safe and non-toxic, the reaction condition is mild, the operation is simple and safe, and the synthesized difluoromethyl modified chiral diamine derivative has good anti-tumor activity and has huge development potential in the field of drug research and development.

The invention belongs to the field of synthetic chemistry and biological medicine, and mainly discloses a difluoromethyl modified polysubstituted chiral tetrahydroquinoline derivative as well as a synthetic method and application thereof. The difluoromethyl modified polysubstituted chiral tetrahydroquinoline derivative is obtained by taking p-toluenesulfonyl difluoromethyl diazomethane, aromatic amine and organic aldehyde as raw materials and taking chiral phosphoric acid as a chiral inducer and an organic reagent as a solvent through a one-step reaction under the catalysis of metal iron. The raw materials are cheap, easy to obtain, safe and non-toxic, the reaction condition of the synthesis method is mild, the operation is simple and safe, and the synthesized difluoromethyl modified polysubstituted chiral tetrahydroquinoline derivative has excellent anti-tumor activity and has bright application prospects in the field of drug research and development.