Chloral hydrate mixture

Fit a 1500 ml. bolt-head flask with a reflux condenser and a thermometer. Place a solution of 125 g. of chloral hydrate in 225 ml. of warm water (50-60°) in the flask, add successively 77 g. of precipitated calcium carbonate, 1 ml. of amyl alcohol (to decrease the amount of frothing), and a solution of 5 g. of commercial sodium cyanide in 12 ml. of water. An exothermic reaction occurs. Heat the warm reaction mixture with a small flame so that it reaches 75° in about 10 minutes and then remove the flame. The temperature will continue to rise to 80-85° during 5-10 minutes and then falls at this point heat the mixture to boiling and reflux for 20 minutes. Cool the mixture in ice to 0-5°, acidify with 107-5 ml. of concentrated hydrochloric acid. Extract the acid with five 50 ml. portions of ether. Dry the combined ethereal extracts with 10 g. of anhydrous sodium or magnesium sulphate, remove the ether on a water bath, and distil the residue under reduced pressure using a Claiseii flask with fractionating side arm. Collect the dichloroacetic acid at 105-107°/26 mm. The yield is 85 g. 

An intimate mixture of betaine hydrate (67.5 g) and chloral hydrate (100 g) was warmed to ca. 60°C when an exothermic reaction occurred and the mixture became pasty. It was then stirred at 60°C for 30 minutes. The residue solidified on cooling and was crystallited from a small amount of water. The product separated in hard, colorless prisms of MP 122.5° to 124.5°C (corr). 

Compound listed in this column added to mixture of other reactants. b Chloral ethylate used in place of free chloral in this reaction. c Chloral hydrate used in place of free chloral in this reaction. d 60 ml. of 20% fuming H2SO4 added during course of reaction. e 50 ml. of fuming H2SO4 added during course of reaction. 

Procedure Weigh accurately about 4 g of chloral hydrate and dissolve in 10 ml of DW and add 30 ml of N sodium hydroxide solution. Allow the resulting mixture to stand for 2 minutes, and then titrate with N sulphuric acid, employing phenolphthalein solution as indicator till a colour change from pink to colourless is achieved. Titrate the neutralized liquid thus obtained with 0.1 N silver nitrate using potassium chromate solution as indicator till precipitation of red chromate is obtained, Add, now 2/15th of the amount of 0.1 N silver nitrate used to the amount of N sulphuric acid used in the first titration and deduct the figure so obtained... 

Chloral Hydrate. Mix chloral with one fifth its weight of water and the mixture slowly solidifies to a crystalline mass of chloral hydrate. 

Due to its Lewis acidic properties, the use of chloral (trichloroacetaldehyde) in the Beckmann rearrangement was investigated . When a variety of ketoximes is admixed with chloral hydrate and the mixture is heated at low pressure in nitrogen atmosphere, the Beckmann rearrangement afforded the corresponding amides in excellent yields (73-98%). The transformation occurs under neutral, relatively mild and solvent-free conditions. 

Chloral hydrate, glutethimide, and methaqualone also produce a depressant effect. Chloral hydrate is dangerous to use as an anesthetic, but it has been used to treat persons undergoing withdrawal from heroin, GHB, and alcohol. A mixture of chloral hydrate and alcohol is termed a Mickey Finn and has been used as a date rape drug. 

Phenol Antimicrobial preservative disinfectant (not oral) Camphor, menthol, thymol, acetaminophen, phenacetin, chloral hydrate, phenazone, ethyl aminobenzoate, methenamine, phenyl salicylate, resorcinol, terpin hydrate, sodium phosphate, or other eutectic formers. Phenol also softens cocoa butter in suppository mixtures... 

Heating a mixture of 6,7,8,9-tetrahydro-ll//-pyrido[2,l-b]quinazolin-ll-one (7) and acetyl and benzoyl chlorides, acetic anhydride, and vinyl acetate under reflux gave 6-condensation products (123), whereas reactions with ethyl chloroacetate, ethyl dichloroacetate, and chloral hydrate afforded 6-substituted products (124) (86MI7). 6,7,8,9-Tetrahydro-ll//-pyrido[2,l-b]quinazolin-l 1-one (7) and acetic anhydride, heated under reflux for 36 h, gave compound 123 (X = OAc, R = Me or X = Me, R = OAc, 18%) and its 6-acetyl derivative (124, R = COMe) in 31% yield (87JHC175 91JHC2071). 

Weak-chlorinated oil from the prechlorinator continuously moves under the distribution graphite grate into the lower part of bubble tower 1. There, at 88-92 °C ethyl alcohol is further chlorinated to reach the density of the chlorinated product of 1.48-1.50 g/cm3. Chlorination extracts a great deal of heat, the excess of which is withdrawn in the tower due to the evaporation of chloral hydrate formed (its boiling point is much lower than that of other components of the reactive mixture). 

Disposition in the Body. After administration, dichloralphenazone acts as a mixture of chloral hydrate and phenazone and reference should be made to the entries under these substances. 

A mixture of 300 g. (1.8 moles) of chloral hydrate and 550 g. of 15% aqueous hydrogen cyanide solution (3.0 moles HCN) is heated in an evaporating dish on a boiling water bath Caution—Hood) until a small test portion of the mixture solidifies on cooling. This should require about 4 hours of heating. The cooled reaction mixture is dried on a clay plate. The product weighs 252 g. (71%) and melts at 58-61° without further purification. 

A mixture of 165 g. (1.0 mole) of chloral hydrate and 202 g. (2.2 moles) of toluene is cooled in an ice bath and stirred vigorously while 6(X) g. of concentrated sulfuric acid is added slowly. The mixture is stirred for 3 hours after completion of the addition and then is poured into crushed ice. The organic product is separated, washed with water, and then triturated with 200 ml. of ethanol. The resulting solid is recrystallized from 1.3 1. of ethanol to give a 53% yield (166 g.) of l,l,l-trichloro-2,2-bis-(p-tolyl)-ethane as white platelets, m.p. 89°. 

Phenyl Salicylate. Phenyl salicylate, salol. occurs as fine white crystals or a white crystalline powder with a characteristic taste and a faint, aromatic odor. It is insoluble in water (1 6.700). slightly soluble in glycerin, and soluble in alcohol (1 6). ether, ehlorofomi. aeetone. or fixed and volatile oils. Dump or eutectic mixtures form readily with many organic material.s. such as thymol, rtrcnthol. camphor, chloral hydrate, and phenol. 

When the chloral hydrate is melted, it and the sulfuric acid are stirred thoroughly and part of the mixture is poured Into the 600 ml beaker and put over the alcohol lamp. Don t let the mixture in the beaker get over 200 F as it will begin to boil away at 210 F. This is where the thermometer comes into play. 

As the mixture heats up, the still impure chloral hydrate will rise to the surface in the beaker, l en it stops rising, take the basting syringe and collect it off the top of the sulfuric acid. It doesn t matter if you pick up a little sulfuric add as long as you get all the chloral hydrate. Store it in the water s. ... 

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... 

---