Magnesium isopropyl- chlorid

Since magnesium becomes bonded to the same carbon that previously held halogen, the alkyl group remains intact during the preparation of the reagent. Thus /1-propyl chloride yields H-propylmagnesium chloride, and isopropyl chloride yields isopropylmagnesium chloride. 

CLORURO de ISOPROPILO (Spanish) (75-29-6) see isopropyl chloride. CLORURO MAGNESICO (Spanish) (7786-30-3 anhydrous 7791-18-6 hexahydrate) see magnesium chloride. CLORURO MERCURICO (Spanish) (7487-94-7) see mercuric chloride. CLORURO de MERCURIO y AMONIO (Spanish) (10124-48-8) see mercury ammonium chloride. 

Isopropyl Chloride 75-29-6 Magnesium Sulfite 7757-88-2 Methyl Carbitol 111-77-3... 

Triaryl phosphates are produced by reaction of phosphoms oxychloride with phenoHc compounds at 100—200°C with magnesium or aluminum chloride catalyst. Past use of cresols and xylenols from coal tar or petroleum is replaced for lower toxicity and cost by synthetic phenoHcs, primarily isopropyl phenol, /-butyl phenol, and phenol itself A range of viscosities is achieved by selection and proportioning of the phenols and their isomers used for the starting material. 

Preparation of 4-aza-S-(N-methyl-4-piperidyll-10,11-dihydro-SH-dibenzo[a,d]cycloheptene-S-ol Add 17.4 g of N-methyl-4-chloropiperidine to a stirred mixture containing 3.2 g of magnesium, 20 ml of anhydrous tetrahydrofuran, 1 ml of ethyl bromide and a crystal of iodine. Reflux for two hours, cool to 30°-35°C and add a solution of 13 g of 4-aza-10,11 -dihydro-5H-dibenzo[a,d] cycloheptene-5-one in 25 ml of tetrahydrofuran. Stir for five hours, remove the solvent by distillation in vacuo and add 250 ml of ether. Add 100 ml of 10% ammonium chloride solution and extract the mixture with chloroform. Concentrate the chloroform solution to a residue and recrystallize from isopropyl ether obtaining 20 g of the carbinol,... 

The mixture was added to 850 cc of water-ice mixture and 82 cc of hydrochloric acid were added thereto. The mixture was extracted with methylene chloride and the combined extracts were washed with water until the wash waters were neutral, were dried over magnesium sulfate and distilled to dryness to obtain 8.480 g of crude product which is purified by crys-tallion from isopropyl ether to obtain 5.810 g of 1 7O -methyl-19-nor-A -pregnadiene-3,20-dione melting at 106°C. 

This reaction mixture is kept between 0°C and -i-5°C for six hours, with agitation and under an inert atmosphere, then 5 cc of a 0.2N solution of acetic acid in toluene are added. The mixture is extracted with toluene, and the extracts are washed with water and evaporated to dryness. The residue is taken up in ethyl acetate, and then the solution Is evaporated to dryness in vacuo, yielding a resin which is dissolved in methylene chloride, and the solution passed through a column of 40 g of magnesium silicate. Elution is carried out first with methylene chloride, then with methylene chloride containing 0.5% of acetone, and 0.361 g Is thus recovered of a crude product, which is dissolved in 1.5 cc of isopropyl ether then hot methanol Is added and the mixture left at 0°C for one night. 

The methyl benzoate thus formed is eliminated by steam distillation, and 2.140 g of crude product are obtained, which are dissolved in 20 cc of methylene chloride. This solution is passed through 10 parts of magnesium silicate, elution being performed with 250 cc of methylene chloride containing 5% of acetone. After evaporation of the solvent 2.050 g of product is recovered, which is recrystallized from isopropyl ether. 

Since sodium borohydride usually does not reduce the nitrile function it may be used for selective reductions of conjugated double bonds in oc,/l-un-saturated nitriles in fair to good yields [7069,1070]. In addition some special reagents were found effective for reducing carbon-carbon double bonds preferentially copper hydride prepared from cuprous bromide and sodium bis(2-methoxyethoxy)aluminum hydride [7766], magnesium in methanol [7767], zinc and zinc chloride in ethanol or isopropyl alcohol [7765], and triethylam-monium formate in dimethyl formamide [317]. Lithium aluminum hydride reduced 1-cyanocyclohexene at —15° to cyclohexanecarboxaldehyde and under normal conditions to aminomethylcyclohexane, both in 60% yields [777]. 

This peracetic acid dispersion is added dropwise to a solution of 11.5 gm (0.1 mole) of 2-isopropyl-3,3-dimethyloxazirane (prepared by the reaction of peracetic acid with A-isopropylideneisopropylamine [75]) in 30 ml of methylene chloride which is cooled in an ice bath. The reaction mixture is allowed to warm to room temperature and is preserved for 16 hr. Then the mixture is treated with 100 ml of cold 20% aqueous ammonia. The organic layer is separated and dried with anhydrous magnesium sulfate. 

The reaction of 6-methylpyridine-3-carboxylic acid methyl ester with N,0-dimethylhydroxylamine and isopropyl-magnesium chloride in toluene gives the N-methoxyamide derivative (x), which is reduced with diisobutyl aluminium hydride (DIBAL) to afford 6-methylpyridine-3-carbaldehyde (xi). The reaction of the aldehyde (xi) with a phosphite provides the diphenyl phosphonate derivative, which is condensed with 4-(methylsulfonyl)benzaldehyde in the presence of potassium fe/f-butoxide in HF to yield the enimine (xii). Finally, this compound is hydrolyzed with HCI to yield the ketosulfone (ix). 

Pinacol possesses the unusual property of forming a crystalline hexahydrate, m.p. 45°, and the pinacol is separated in this form from the unreaoted acetone and the isopropyl alcohol. The magnesium is conveniently amalgamated by dissolving mercuric chloride in a portion of the. acetone mercury is then liberated by the reaction ... 

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