45 results about "Methylmagnesium chloride" patented technology

The present invention discloses a montelukast sodium preparation technology and intermediates; 7-chloro-2-methylquinine and 3-bromobenzaldehyde are used as raw materials for condensation reaction to obtain a compound A2; by carbon-carbon coupling of the compound A2 and 1-tetralone in the presence of a catalyst, an intermediate compound A3 is obtained; an important intermediate compound A4 is obtained by bio-enzyme catalyzed asymmetric Baeyer-villiger reaction, a chiral center is highly selectively constructed, an important intermediate compound A5 is prepared from the compound A4 by grignard reaction by use of methylmagnesium chloride, finally montelukast sodium (A6) is obtained; according to the technology, the highly chiral important intermediate compound A4 is obtained by bio-enzyme catalyzed asymmetric reaction, the catalyst can be effectively repeatedly used, and the kind of used solvents is less, and the montelukast sodium preparation technology has the characteristics of safety and environmental protection, greatly saves the production cycle, is low in production cost, high in total yield, and simple in operation of production units, and is suitable for industrialized production.

The invention relates to a Ziegler-Natta polyethylene catalyst loaded by double carriers of magnesium chloride / mesoporous molecular sieve, a preparation method and an application thereof. The catalyst is made up by taking titanium tetrachloride as a main catalyst of active components and organic aluminum as a cocatalyst. The double carriers of the magnesium chloride / mesoporous molecular sieve aretaken as a carrier; an organic reagent of magnesium is used, by the breaking and creation of chemical bonds, Si-O-Mg bond is generated so as to obtain a complex carrier with clear structure. The dried mesoporous molecular sieve is suspended in toluene and added with tetrahydrofuran solvent of methyl magnesium chloride; the methyl magnesium chloride on a surface is reacted with silanol group to form the Si-O-Mg bond; and an obtained complex carrier has the frame of the mesoporous molecular sieve and the surface of the magnesium chloride, and can possess the advantages of the double carriers. The active titanium is loaded on the double carriers of chloride / mesoporous molecular sieve to catalyze the polymerization of ethane, thereby obtaining polyethylene with a super molecular weight of 600thousand to 7 million.

The invention provides a preparation method of a metandienone product. The preparation method comprises the following steps that 1,4-androstenedione, namely IDD, is adopted as a raw material, in the presence of methylmagnesium chloride, an organic solvent and acid, alpha-CH3 and beta-OH are introduced at the 17 position, and metandienone is prepared; and then the obtained metandienone is heated byactivated carbon in acetone or lower alcohol below C4 for reflow discoloration and is recrystallized, and the metandienone product is obtained. According to the preparation method, the IDD serves asthe raw material to prepare the metandienone, compared with a traditional method adopting diosgenin as a raw material, the raw material source is wide, a process is economic and environmentally friendly, and the production cost is significantly lowered. Compared with a traditional production method, according to the preparation method, a synthesis route is short, the process is easy, convenient and environmentally friendly, the product yield is high, the quality is good, and the production raw material cost is lowered by 40-45% by calculating through the current raw material price.

The present invention discloses a method for preparing 2,3,3,3-tetrafluoropropene using methylmagnesium chloride, comprising the following steps: 1) preparing 1,1,2-trifluoropropene (CH3CF═CF2); 2) preparing 1,1,1,2,2-pentafluoropane (CF3CF2CH3); 3) preparing 2,3,3,3-tetrafluoropropene (CF3CF═CH2). In the present invention, using a Grignard reagent, namely methylmagnesium chloride, and tetrafluoroethylene as starting raw materials, 2,3,3,3-tetrafluoropropene is prepared by three steps of nucleophilic addition-elimination, fluorine addition, and dehydrofluorination in sequence. The process flow is relatively short, and the product yield is high.

The invention discloses a continuous flow method for preparing an intermediate of olmesartan medoxomil, which belongs to the technical field of pharmaceutical synthesis and comprises the following steps: step (1), compounding formula I compound 2-propyl-4,5-imidazole dicarboxylic acid Ethyl ester I is dissolved in organic solvent to form reaction phase A, step (2), the methylmagnesium chloride solution of commercialization purchase is used as reaction phase B, step (3), reaction phase A and reaction phase B are used plunger pump to Pump it into the mixer at a certain flow rate, then enter the reactor, keep it for a certain period of time, quench it with the acidic water phase C, and enter the oil-water continuous separator for liquid separation, that is, the organic solution of the compound formula II is obtained. The compound of formula II can be obtained by recrystallization, which solves the technical problems of low purity and high cost in the existing production process. The product of the present invention has high purity and few impurities, and the content of key impurity A, key impurity B and key impurity C can be controlled at 0.1 % or less, and the raw materials are cheap and easy to obtain, the reaction conditions are mild, the operation is simple, the synthesis efficiency is high, and it is suitable for industrial production. It provides a new continuous flow route for the preparation of olmesartan medoxomil and intermediates.

The invention discloses a method for synthesizing trimethylphosphine oxide and belongs to the field of compound preparation. The method includes: under nitrogen protection, allowing chloromethane and magnesium chips to react in the mixed solution of toluene and tetrahydrofuran by using bromoethane as initiator so as to obtain methylmagnesium chloride; directly adding trichlorine into the methylmagnesium chloride, which needs not to be purified, after cooling, stirring under low temperature to allow for reaction, extracting after the reaction is completed, and performing vacuum refinery distillation and cooling crystallization to obtain the trimethylphosphine oxide. The method has the advantages that the purity of the obtained trimethylphosphine oxide is above 99.5%, the yield of the trimethylphosphine oxide reaches 95%, and the solvent used by the method is easy to recycle.

The invention discloses a preparation method of ethoxyquin. The method comprises the following concrete steps: 1, enabling 4-ethoxy-N-(propane-2-alkenyl)aniline, which is taken as a raw material, to react with ((2-methyl-1,3-dioxolane-2-yl)methyl)magnesium chloride to obtain an intermediate product; 2, hydrolyzing the obtained intermediate product for deprotection; 3, enabling the hydrolyzed product to make a cyclization reaction under an acidic condition to prepare the ethoxyquin. The ethoxyquin is prepared by a one-step method, the intermediate produced in the preparation process does not need to be separated, and a great deal of acetone and methylbenzene are not needed by the reaction, so that the conversion rate of the raw material is better improved, a reaction solvent is saved, and the pressure of environmental protection is reduced; the preparation method has the advantages of mild reaction conditions, simple technology, convenient operation and environment friendliness; furthermore, the obtained product is also higher in purity and can meet the demands of feed markets at all levels, thus having better industrial prospect.