Magnesium dimethyl

N-Phenacyl-N -methylpiperazine Cyclohexyl bromide Magnesium Dimethyl sulfate... 

Magnesium dimethyl, Mg(CH3)2, may be prepared by heating magnesium turnings with mercury dimethyl for thirty-six hours at 130° C. It is described as a grey-yellow mass, which reacts vith explosive violence with water. The addition of acetyl chloride to a well-cooled ethereal solution of the compound in a nitrogen atmosphere... 

Me2NCH2) C2H5)(Me)C-OOC Ph-HCI. Colourless crystalline powder with a bitter taste, m.p. 177-179"C. Prepared by the action of ethyl magnesium bromide on dimethyl-aminoaceione. It is a local anaesthetic, mainly used to produce spinal anaesthesia. 

Dimethyl n-propyl carbinol, CH3(CH2)2COH(CH3)2. From n-propyl magnesium bromide and acetone. Collect the tertiary alcohol at 121-124°. 

Dimethyl ethyl carbinol (2-methy 1-2-butanol or amyl alcohol), CH3CHjCOH(CH3).2. From ethyl propionate and methyl magnesium iodide. Collect the tertiary alcohol at 100-102°. 

Di lve 20 g. of the cyano ester in 100 ml. of rectified spirit and add a solution of 19 2 g. of pure potassium cyanide in 40 ml. of water. Allow to stand for 48 hours, then distil oflF the alcohol on a water bath. Add a large excess of concentrated hydrochloric acid and heat under reflux for 3 hours. Dilute with water, saturate the solution with ammonium sulphate, and extract with four 75 ml. portions of ether. Dry the combined ethereal extracts with anhydrous sodium or magnesium sulphate, and distil off the ether. RecrystaUise the residual acid from excess concentrated hydrochloric acid, and dry in the air. The yield of pure ew-dimethyl-succinic acid, m.p. 141-142°, is 12 g. 

Add the dimethyl sulphate dropwise during 1 hour whilst stirring the mixture vigorously. Then reflux for 2 hours, with stirring, in order to complete the methylation. Allow to cool, add water, transfer to a separatory funnel, remove the lower layer, and wash once with water, twice with dilute sulphuric acid, and then with water until the washings are neutral to litmus. Add some sodium chloride to each washing as this will facilitate the separation of the two layers for anisole is 0- 996). Dry over anhydrous calcium chloride or magnesium sulphate, and distil from an air bath. Collect the anisole at 151-154°. The yield is 40 g. 

Myristic acid from hexanoic acid and methyl hydrogen sebacate). Dissolve 23 -2 g. of redistilled hexanoic acid (re caproic acid), b.p. 204-6-205-5°/760 mm., and 21-6 g. of methyl hydrogen sebacate in 200 ml. of absolute methanol to which 0 13 g. of sodium has been added. Electrolyse at 2 0 amps., whilst maintaining the temperature between 30° and 40°, until the pH is about 8 0 (ca. 6 hours). Neutralise the contents of the electrolysis cell with a little acetic acid and distil off the methyl alcohol on a water bath. Dissolve the residue in 200 ml. of ether, wash with three 50 ml. portions of saturated sodium bicarbonate solution, once with water, dry with anhydrous magnesium sulphate, and distil with the aid of a fractionating column (see under Methyl hydrogen adipate). Collect the re-decane at 60°/10 mm. (3 0 g.), the methyl myristate at 158-160°/ 10 mm. (12 5g.) and dimethyl hexadecane-1 16-dicarboxylate at 215-230°/ 7 mm. (1 -5 g.)... 

Exp. 4) with cooling to about -20°C. The addition was carried out in about 10 min. Ten minutes later the solution was cooled to -60°C and a mixture of 0.20 mol of dimethyl disulfide and 50 ml of diethyl ether was added in 15 min with efficient cooling, so that the temperature could be kept below -40°C. Five minutes after the addition the mixture was poured into ice-water and three extractions with diethyl ether were carried out. The combined solutions were dried over magnesium sulfate and concentrated in a water-pump vacuum. Distillation of... 

Organomineral peroxides of antimony arsenic, boron, magnesium, tin, cadmium, lead, silicon, and 2inc have been prepared by autoxidation and some are Hsted in Table 3 (33,44,60,93,115). For example, dimethyl cadmium reacts with oxygen to form methylperoxy methyl cadmium [69331-62-0] and bis(methylperoxy) cadmium. 

In some instances a carbon-carbon bond can be formed with C-nucleophiles. For example, 3-carboxamido-6-methylpyridazine is produced from 3-iodo-6-methylpyridazine by treatment with potassium cyanide in aqueous ethanol and l,3-dimethyl-6-oxo-l,6-dihydro-pyridazine-4-carboxylic acid from 4-chloro-l,3-dimethylpyridazin-6-(lH)-one by reaction with a mixture of cuprous chloride and potassium cyanide. Chloro-substituted pyridazines react with Grignard reagents. For example, 3,4,6-trichloropyridazine reacts with f-butyl-magnesium chloride to give 4-t-butyl-3,5,6-trichloro-l,4-dihydropyridazine (120) and 4,5-di-t-butyl-3,6-dichloro-l,4-dihydropyridazine (121) and both are converted into 4-t-butyl-3,6-dichloropyridazine (122 Scheme 38). 

The most common impurities are the corresponding acid and hydroxy compound (i.e. alcohol or phenol), and water. A liquid ester from a carboxylic acid is washed with 2N sodium carbonate or sodium hydroxide to remove acid material, then shaken with calcium chloride to remove ethyl or methyl alcohols (if it is a methyl or ethyl ester). It is dried with potassium carbonate or magnesium sulfate, and distilled. Fractional distillation then removes residual traces of hydroxy compounds. This method does not apply to esters of inorganic acids (e.g. dimethyl sulfate) which are more readily hydrolysed in aqueous solution when heat is generated in the neutralisation of the excess acid. In such cases, several fractional distillations, preferably under vacuum, are usually sufficient. 

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