6 results about "Borane dimethylsulfide" patented technology

The invention discloses a tetra-coordinated boron-oxygen heterocyclic compound and a preparation method thereof, and belongs to the technical field of pharmaceutical and chemical intermediates and related chemistry. The method comprises the following steps: by taking a bis (pentafluorophenyl) borane dimethyl sulfide complex [(C6F5) 2BHSMe2] as a boron source, firstly carrying out hydroboronation reaction on the bis (pentafluorophenyl) borane dimethyl sulfide complex [(C6F5) 2BHSMe2] and an eneyne compound to generate a three-coordination alkenyl boron dienophile intermediate in situ, and then carrying out reverse electron demand Diels-Alder reaction on the three-coordination alkenyl boron dienophile intermediate and an acetylenic ketone compound to synthesize a series of tetra-coordination boron-oxygen heterocyclic compounds. The method has the advantages of mild reaction conditions, good selectivity, high yield, wide substrate application range, environmental friendliness, simplicity and convenience in operation and the like, opens up a new way for synthesis of the tetra-coordinated organoboron compound, and has higher application value and social and economic benefits.

The invention provides a synthetic method of borneol, and belongs to the field of medicine synthesis. According to the preparation method, natural camphor is taken as a starting material, (R)-2-methyl-CBS-oxazole borane is taken as a chiral catalyst, borane dimethyl sulfide tetrahydrofuran is taken as a reducing agent, and reaction is carried out in an organic solvent to synthesize borneol, the invention relates to a medicine composition for preventing and treating ovarian cancer, which is prepared from the following raw materials in parts by mole: 328.44 parts of camphor, 16.42 parts to 295.59 parts of (R)-2-methyl-CBS-oxazole borane and 328.44 parts to 591.18 parts of borane dimethyl sulfide tetrahydrofuran. The medicine composition is prepared from the following raw materials in parts by mole: 38.44 parts of camphor, 16.42 parts to 295.59 parts of (R)-2-methyl-CBS-oxazole borane and 38.44 parts to 591.18 parts of borane dimethyl sulfide tetrahydrofuran. According to the synthetic method disclosed by the invention, on the premise of using a small amount of the chiral catalyst, the reaction time is obviously shortened, the method is high in reproducibility, strong in magnification and stable in yield, and the product quality is obviously superior to the quality standard of natural borneol.

This invention belongs to the field of chemical synthesis technology, specifically relating to a method for synthesizing 1-(7-amino-6-bromo-4,4-dimethyl-3,4-dihydroquinoline-1(2H)-yl)ethyl-1-one. Using compound A as a basic raw material, this invention obtains 1-(7-amino-6-bromo-4,4-dimethyl-3,4-dihydroquinoline-1(2H)-yl)ethyl-1-one through reactions such as reaction with borane dimethyl sulfide, nitration, and acetylation. This method is easy to operate and produces products with high yield and high purity.

The invention belongs to the technical field of material synthesis, and particularly relates to bis (tetramethylammonium dodecahydrododecaborate) as well as a synthesis method and application thereof. According to the synthesis method of the dodecahydrododecaborate bis (tetramethylammonium), expensive and difficult-to-obtain raw materials are not used, the dodecahydrododecaborate bis (tetramethylammonium) is synthesized through one-step reaction of tetramethyl ammonium borohydride (CH3) 4NBH4 and the borane dimethyl sulfide complex in the high-pressure reaction kettle, the reaction steps are simple, the yield is high, and the method is suitable for industrial production. According to the present invention, the dodecahydrododecaboronic acid bis (tetramethyl) ammonium synthesis process has characteristics of high yield and high purity, is an efficient dodecahydrododecaboronic acid bis (tetramethyl) ammonium synthesis process, is hopeful to provide the high-purity dodecahydrododecaboronic acid bis (tetramethyl) ammonium on a large scale, meets the application requirements of dodecahydrododecaboronic acid bis (tetramethyl) ammonium in a plurality of fields, and has wide application prospects. Therefore, the technical problem that an efficient synthesis process for dodecahydrododecaboronic acid bis (tetramethylammonium) is lacked at present is solved.

The invention discloses a ruthenium complex precursor synthesis method, which comprises: adding a ruthenium trichloride hydrate (112.8 g, 0.41 mol) with a ruthenium content of 37% and 1.6 L of ethanol into a 5000 ml multi-port reaction bottle under a nitrogen atmosphere, and stirring to dissolve; dropwise adding pyridine (163.3 g, 2.06 mol) into a reaction system at room temperature, after dropwise adding is completed, heating to reflux and reacting for 3 hours until the system becomes red, slowly recovering to room temperature, and filtering; the preparation method comprises the following steps: adding a sodium acetate solution into a reaction kettle, stirring, filtering, concentrating filtrate to 2 / 3 of the volume, cooling to 0 DEG C, dropwise adding a tetrahydrofuran solution of sodium acetylcyclopentadienyl (820 mL, 0.82 mol) with the molar concentration of 1 mol / L, slowly recovering to room temperature after dropwise adding, continuously reacting for 10 hours, draining the solvent, extracting by using dichloromethane, filtering, draining the filtrate, pulping a crude product by using ethanol, filtering, washing by using ethanol, and drying to obtain a finished product. 91.8 g of the diacetyl ruthenium dicyclopentadienyl intermediate is obtained, and the yield is 71%; and borane dimethyl sulfide reduction is carried out. The method has the advantages of simple and easily available reaction raw materials, convenient operation, mild reaction conditions, low cost and high safety coefficient.

The invention provides a preparation method of 3-fluoro-4-chlorobenzyl bromide, which comprises the following steps: (1) carrying out low-temperature reaction on 4-chloro-3-fluorobenzoic acid and a borane dimethyl sulfide complex in a solvent to obtain an intermediate I; and (2) reacting the intermediate I obtained in the step (1) with phosphorus tribromide in dichloromethane to obtain the 3-fluoro-4-chlorobenzyl bromide. The yield of the first step of the reaction can reach 95% or above, the purity reaches 98%, the yield of the second step of the reaction can also reach 95% or above, the purity reaches 98% or above, and compared with an existing route, the yield and the purity are higher, and the method is suitable for mass production and has high application value.