Calcium sulfate mole fraction

A mixture of 171 g. (1 mole) of dimethyl-a-naphthylamine (Note 1) and 125 g. (1.2 moles) of cyanogen bromide 1 in a 1-1. flask (Note 2) is heated under reflux on the steam bath for 16 hours (Note 3). The cooled reaction mixture is added to 2.5 1. of dry ether, and the insoluble quaternary salt (Note 4) is filtered. The ether filtrate is extracted with four 800-ml. portions of approximately 15% hydrochloric acid solution (Note 5) and washed with five 500-ml. portions of water. The ether solution is dried with 30-35 g. of anhydrous calcium sulfate (Drierite). After filtration, the solvent is removed by distillation at atmospheric pressure on the steam bath the residue is fractionated under reduced pressure. The yield of pale yellow oil, boiling at 170-171°/ mm- (185—187°/3 mm.), amounts to 115-122 g. (63-67%) (Note 6). 

B) Epibromohydrin.—In a 5-I. round-bottomed flask, 2140 g. (1000 cc., 9.8 moles) of glycerol a ,t-dibromohydrin (Org. Syn. 14, 42) is suspended in 1.5 1. of water, and 400 g. of technical, powdered calcium hydroxide (88 per cent) is added gradually, with shaking, in the course of about fifteen minutes. A further quantity of 400 g. of calcium hydroxide (total, 10 moles) is added at once, and the epibromohydrin is distilled at reduced pressure in the manner described for epichlorohydrin (Note 2). The combined lower layers from two such distillations (about 750 cc.) are dried over anhydrous sodium sulfate and fractionated at atmospheric or reduced pressxue. The yield of epibromohydrin, b.p. 134-136° or 6i-62°/5o mm., is 1130-1200 g. (84-89 per cent of the theoretical amount). 

Step B. To the aqueous reaction mixture described under Step A is added 1000-1500 ml. of methanol and the mixture is allowed to stand at room temperature for three hours. The dimethylal and methanol are then distilled out, distillation being stopped when the temjierature of the residue reaches 90°. The mixture is cooled and treated with 10 moles of 40% sodium hydroxide. The amine layer is taken up in ether and the aqueous layer extracted three times with 300 ml. of ether. The ether extract is dried Over anhydrous calcium sulfate and the ether is then removed by distillation. Distillation of the amine is carried out from a Claisen flask, b.p. 82° at 17 mm., 1.5615. Further purification can be effected by distillation through a 12-plate fractionating column. 

Wang et al. 146) reported in 1956 the isolation of succinate dehydrogenase from heart muscle preparations treated with succinate and cyanide. The enzyme was extracted with 20% aqueous ethanol at pH 9.0. The final product, after adsorption on calcium phosphate gel and ammonium sulfate fractionation, was stated to be electrophoretically homogeneous and to contain 1 mole of flavin and 4 g-atoms of iron per 140,000-... 

A SOLUTION of 250 g. (1.51 moles) of chloral hydrate (Note i) in 450 cc. of warm water (50-60°) is placed in a 3-I. round-bottomed flask bearing a reflux condenser and thermometer (Note 2). The condenser is temporarily removed and 152.5 g. (1.52 moles) of precipitated calcium carbonate added this is followed by 2 cc. of amyl alcohol (Note 3) and a solution of 10 g. of sodium cyanide (Note 4) in 25 cc. of water. Althou the reaction is exothermic, the reaction mixture is heated with a low flame so that it reaches 75° in about ten minutes at this point heating is discontinued. The temperature continues to rise to 80-85° during five to ten minutes and then drops. As soon as the temperature begins to fall the solution is heated to boiling and refluxed for twenty minutes. The mixture is then cooled to 0-5° in an ice bath, acidified with 215 cc. of concentrated hydrochloric acid (sp. gr. 1.18) and extracted with five loo-cc. portions of ether (Note 5). The combined ether extracts are dried with 20 g. of anhydrous sodium sulfate, the ether is removed by distillation from a steam bath, and the residue distilled in vacuum from a Claisen flask with a fractionating side... 

Distilled ethyl oleate (200 g, 0.65 mole) and absolute alcohol (1.51) are placed in a 5-1 round-bottomed flask under a wide reflux condenser. The alcohol has been previously dried over calcium and is distilled from aluminum ferf-butoxide directly into the reaction flask. Sodium (to a total of 80 g, 3.5 gram-atoms) is added gradually through the reflux condenser at such a rate that vigorous reaction ensues, the flask being occasionally shaken. When the main reaction has ended, more absolute alcohol (200 ml) is added and the mixture is heated on the steam-bath until all the sodium is consumed. Then water (500 ml) is added and the heating continued for a further hour to hydrolyse unchanged ester. The imsaponifiable fraction is extracted with ether. The ether extract is washed with 1 % potassium hydroxide solution and then with water until free from alkali (phenolphthalein) and is dried over sodium sulfate. The ether is distilled off and the residue is fractionally distilled. 49-51 % (84-89 g) of oleyl alcohol are obtained at 150-152°/1 mm. 

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