3 results about "Methylmagnesium chloride" patented technology

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 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.