12 results about "Methylmagnesium chloride" patented technology

The present invention belongs to the technical field of the preparation of organic compounds, and particularly relates to a method for preparing crotyl alcohol in multiple steps using epichlorohydrin as a raw material. The method for preparing crotyl alcohol in multiple steps using epichlorohydrin as a raw material according to the present invention comprises the following steps: adding epichlorohydrin to tetrahydrofuran, slowly dropping a tetrahydrofuran solution of methylmagnesium chloride, maintaining the temperature for mixing reaction, and after completion, adjusting the pH to neutral at room temperature, and treating to obtain 3-chloro-2-butanol; slowly adding phosphorus oxychloride to pyridine, cooling in an ice bath, adding the obtained 3-chloro-2-butanol, reacting at room temperature, pouring into an ice-water mixture, and then adjusting the pH to neutral, and treating to obtain 1-chloro-2-butene; adding the obtained 1-chloro-2-butene to a sodium hydroxide solution, heating for reaction, and treating to obtain crotyl alcohol. The method for preparing crotyl alcohol in multiple steps using epichlorohydrin as a raw material provided by the present invention has the advantages of simple operation, mild conditions, low cost, high yield, and good environmental protection performance.

The invention provides a medetomidine preparation method, which comprises: S1, taking 2, 3-dimethyl benzaldehyde as an initial raw material, and carrying out a reaction on the 2, 3-dimethyl benzaldehyde and methylmagnesium chloride to generate 1-(2, 3-dimethyl phenyl) ethanol; s2, excessive silyl group protected imidazole is added into a reaction system in the step S1, and an activated [1-(2, 3-dimethylphenyl) ethyoxyl] silyl ether intermediate is obtained; taking trimethylsilyl trifluoromethanesulfonate as a catalyst, carrying out a Friedel-Crafts reaction with silyl-protected imidazole, and after the reaction is finished, carrying out post-treatment on the reaction liquid to obtain a medetomidine crude product. 2, 3-dimethyl benzaldehyde is adopted as a starting raw material, medetomidine is prepared through a one-pot method, raw materials are cheap, reaction steps are short, the production cost is greatly reduced, TMSOTf is adopted as a catalyst in the Friedel-Crafts reaction, the reaction is efficient, it can be effectively avoided that in the aftertreatment process of a traditional catalyst titanium tetrachloride, a large number of titanic acid colloidal solid insoluble substances are formed, and the yield of medetomidine is increased. The problem that post-treatment layering is difficult is solved, and the yield is increased.

The application belongs to the technical field of dielectric material monomer synthesis, and discloses a preparation method of 1-methylbenzocyclobutene. The application adopts 1-hydroxybenzocyclobutene as raw material, and reacts with p-toluenesulfonyl chloride (TsCl) to generate 1-p-toluenesulfonyloxybenzocyclobutene. Then, the 1-p-toluenesulfonyloxybenzocyclobutene reacts with methylmagnesium chloride under the action of a catalyst to obtain the target product 1-methylbenzocyclobutene. The target product is synthesized under relatively mild conditions mainly by controlling the reaction temperature, the feeding sequence and the feeding ratio. The process operation is simple, the experimental condition is mild, the product yield is high, and the method is suitable for industrial production.

The present application discloses a high-purity organometallic film precursor and a preparation method therefor. The method comprises: under nitrogen protection, loading a metal halide into a flask, adding an ether solvent, and cooling to a temperature A; slowly injecting methylmagnesium chloride into the flask over a set period of time while controlling the reaction temperature to not exceed a temperature B; after injection, raising the reaction temperature to a temperature C and stirring during reflux; upon completion of reflux, cooling the reaction solution back to the temperature A, and slowly adding a prepared Grignard reagent into the reaction solution while controlling the reaction temperature to not exceed the temperature B during the addition; after injection, raising the reaction temperature to the temperature C and stirring during reflux; upon completion of the reaction, separating magnesium chloride by means of vacuum filtration, and removing the solvent by means of filtrate vacuum distillation, to obtain the organometallic film precursor. The present application has the advantages of good process safety, high yield, high product purity, and high preparation efficiency.

The invention relates to the technical field of organic synthesis, and particularly discloses a preparation method of 4-isopropenylphenol, which comprises the following steps: hydroxyl protection: under the action of stirring, adding p-hydroxyacetophenone or p-hydroxybenzaldehyde into a solvent A, then adding a hydroxyl protective agent and alkaline ion exchange resin, carrying out heat preservation reaction at 10-15 DEG C for 3-4 hours, filtering, washing, and drying to obtain 4-isopropenylphenol; filtering, extracting and concentrating to obtain an intermediate 1; grignard reaction: under the stirring action, adding the intermediate 1 into a solvent B, heating to 35-45 DEG C, then dropwise adding a Grignard reagent, continuously carrying out heat preservation reaction for 5-6 hours, after the reaction is finished, adding a hydrochloric acid solution, standing for phase separation, and concentrating to obtain an intermediate 2; the Grignard reagent is isopropyl magnesium chloride or methyl magnesium chloride. According to the preparation method provided by the invention, the 4-isopropenylphenol with the yield being greater than or equal to 60% and the purity being greater than or equal to 98% can be obtained, the reaction operation is simple, and large-scale industrial production is facilitated.

The invention belongs to the technical field of preparation of organic compounds, and particularly relates to a method for preparing crotyl alcohol in multiple steps by taking epichlorohydrin as a raw material. The method for preparing crotyl alcohol in multiple steps by taking epoxy chloropropane as a raw material comprises the following steps: adding epoxy chloropropane into tetrahydrofuran, slowly dropwise adding a tetrahydrofuran solution of methylmagnesium chloride, keeping the temperature, mixing and reacting, adjusting the pH to be neutral at room temperature after the reaction is completed, and treating to obtain 3-chloro-2-butanol; slowly adding phosphorus oxychloride into pyridine, cooling in an ice bath, adding the obtained 3-chloro-2-butanol, reacting at room temperature, pouring into an ice-water mixed solution, regulating the pH value to be neutral, and treating to obtain 1-chloro-2-butene; and adding the obtained 1-chloro-2-butene into a sodium hydroxide solution, heating to react, and treating to obtain the crotonol. The method for preparing crotyl alcohol in multiple steps by taking epichlorohydrin as the raw material provided by the invention is simple to operate, mild in condition, low in cost, high in yield and good in environmental protection property.

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing methylsulfonyl fluoride from byproduct sulfuryl chloride fluorine. The method for synthesizing methylsulfonyl fluoride from byproduct sulfuryl chloride fluorine comprises the following steps: firstly, preparing a methylmagnesium chloride solution; then adding sulfuryl chloride fluorine into the reaction container, cooling to-15 DEG C to 5 DEG C, dropwise adding a methylmagnesium chloride solution while stirring under an anaerobic condition, and carrying out a heat preservation reaction after dropwise adding to obtain a methylsulfonyl fluoride reaction solution; and finally, adding water into the reaction liquid for quenching, standing for liquid separation to obtain a water phase and an organic phase, treating the water phase to obtain magnesium chloride (hexahydrate), and refining the organic phase to obtain methylsulfonyl fluoride. According to the method for synthesizing the methylsulfonyl fluoride from the byproduct sulfuryl chloride fluorine, the treatment problem of the byproduct sulfuryl chloride fluorine is solved, the raw material cost in the synthesis process is low, and the obtained methylsulfonyl fluoride is high in purity and yield.

The invention discloses design, synthesis and activity research of a fluorescent probe for in-situ detection of nitroreductase. The synthesis route of the fluorescent probe is as follows: # imgabs0 # aReagens and bonds: (i) Ethyl iode, KOH and DMF, and the temperature is 90 DEG C; (ii) MethylMagnesite chloride, NaI, THF (tetrahydrofuran), and the temperature is 55 DEG C; (iii) 4-nitrobenzyl bromide, K2CO3, DMF (Dimethyl Formamide), rt, K2CO3, K2CO3, DMF, rt and K2CO3; and (iv) n-Butanol, Toluene, and the temperature is 100 DEG C.

The present invention discloses a method for synthesizing 9,9-dimethyl-2-bromofluorene. The method uses 2-bromo-9-fluorenone and methylmagnesium chloride as raw materials, and further reacts them under the action of zirconium tetrachloride to obtain the final product, 9,9-dimethyl-2-bromofluorene. The method has the advantages of cheap and readily available raw materials, convenient production, and ease of purification, and can be developed into an industrial production method.

The present invention belongs to the technical field of organic synthesis, and in particular to a method for synthesizing methylsulfonyl fluoride from by-product sulfuryl chloride. The method for synthesizing methylsulfonyl fluoride from by-product sulfuryl chloride according to the present invention comprises the following steps: first preparing a methylmagnesium chloride solution; then adding sulfuryl chloride to a reaction vessel, cooling to -15°C~5°C, and adding the methylmagnesium chloride solution dropwise with stirring under anaerobic conditions, and dropping and finishing the insulation reaction to obtain a methylsulfonyl fluoride reaction solution; finally, quenching the reaction solution with water, standing and separating the liquid to obtain an aqueous phase and an organic phase, treating the aqueous phase to obtain magnesium chloride (hexahydrate), and refining the organic phase to obtain methylsulfonyl fluoride. The method for synthesizing methylsulfonyl fluoride from by-product sulfuryl chloride provided by the present invention solves the problem of processing by-product sulfuryl chloride, has low raw material cost during the synthesis process, and has high purity and high yield of the obtained methylsulfonyl fluoride.

The invention discloses an adamantane phosphinamine ligand as well as a preparation method and application thereof, and belongs to the technical field of organic phosphorus compound synthesis, the ligand has the following general formula (I): the preparation method comprises the following steps: reacting 1-adamantanamine with chloro-dicyclohexylphosphine in the presence of methylmagnesium chloride to obtain N-((3s, 5s, 7s)-adamantane-1-yl)-1, 2, 3, 4, 5-tetramethyl-1, 3, 4-tetramethyl-1, 3, 4-tetramethyl-1, 3, 4-tetramethyl-1, 3, 4-tetramethyl-1, 3, 4-tetramethyl-1, 3, 4-tetramethyl-1, the catalyst is 1, 1-dicyclohexylphosphinamine; n-((3s, 5s, 7s)-adamantane-1-yl)-1, 1-dicyclohexylphosphinamine generates phosphinamine anions under the action of alkali, and the phosphinamine anions and alkyl chloride are subjected to an alkylation reaction to obtain rigid phosphinamine ligands of different substitution types. According to the invention, the problems of high structural flexibility, unstable coordination configuration, difficulty in regulation and control of catalytic selectivity and the like of the existing phosphinamine ligand are solved.

This invention discloses a method for preparing 25-hydroxycholesterol, belonging to the technical field of 25-hydroxycholesterol. The method includes: mixing tetrahydrofuran and KGP-06 and cooling to below 0°C under nitrogen protection; then adding methyl magnesium chloride solution dropwise, controlling the reaction temperature below 15°C; continuing to add hydrochloric acid solution to obtain a first reaction solution; pouring the first reaction solution into acidic water, controlling the temperature below 40°C, then concentrating; then adding water and cooling to below 30°C; filtering, washing with water, and drying to obtain a solid; then adding DCM and methanol to dissolve the solid; then concentrating; adding methanol to displace to a viscous state; and then cooling to crystallize to obtain the 25-hydroxycholesterol. This invention uses KGP-06 as a raw material to obtain 25-hydroxycholesterol via Grignard reaction, with a yield as high as 97% and a purity greater than 98%. This preparation method is simple and has a high yield.