Semi-Solids

Vaseline A trade name for soft paraffin. Yellow and white semi-solid, partly translucent mixtures of hydrocarbons of the paraffin series ranging from CijHji to C2oH42- Obtained from the high-boiling fractions of petroleum... 

Dissolve 10 g. of salicylic acid (o-hydroxybenzoic acid) in 7 ml. of dry pyridine contained in a too ml. conical flask. Then without delay (since this solution if allowed to stand tends to become a semi-solid mass) run in 7 5 ml. (8 3 g.) of acetyl chloride, adding about i ml. of the chloride at a time, and shaking the mixture continuously during the addition. The heat of the reaction causes the temperature of the mixture to rise rapidly ... 

Sodium amalgam. The amalgam which is generally employed for reductions contains from 1 to 3 per cent, of sodium. Amalgams with a greater sodium content than 1 2 per cent, are solid at the ordinary temperature and can be powdered in a mortar the 1 2 per cent, amalgam is semi-solid at room temperature but is completely fluid at 50°. Two methods of preparation are available. 

The stirrer used is a bent glass rod which nearly scrapes the sides of the flask. A simple paddle stirrer is not efficient enough to stir the semi-solid mass. 

The flask is placed in an ice-salt mixture and the contents decomposed by the gradual addition of 300 cc. of saturated ammonium chloride solution and 100 cc. of water (Note 4). The aqueous layer is removed by means of a 1500-cc. separatory funnel and sufficient ether is added to dissolve the yellow precipitate. The total volume of ether solution is about one liter. This is washed with two 200-cc. portions of water, and the three aqueous layers are extracted consecutively with a loo-cc. portion of ether. The combined ether solution is dried over 30 g. of anhydrous sodium sulfate, coricentrated on the steam bath to a volume of about 200 cc., and cooled to room temperature. The product which crystallizes is collected with suction and washed with two 25-cc. portions of ether. The yield is 35-38 g. of light yellow product, m.p. 122-123°. The ether is completely removed from the combined filtrates by heating on the steam bath, and the black oil is allowed to stand overnight. The semi-solid mass is filtered with suction and washed with a minimum amount of cold ether. In this way an additional 6-7 g. of yellow material is obtained which melts at 119-121°. 

In a 3-I. round-bottomed flask 250 g. of commercial calcium hypochlorite is dissolved in i 1. of warm water and a warm solution of 175 g. of potassium carbonate and 50 g. of potassium hydroxide in 500 cc. of water is added. The flask is stoppered and shaken vigorously until the semi-solid gel which first forms become quite fluid. The suspended solid is removed by filtration on a large Buchner funnel, washed with 200 cc. of water, and sucked as dry as possible with the aid of a rubber dam and an efficient suction pump. The filtrate of approximately 1500 cc. is placed in a 3-I. round-bottomed flask and is ready for the addition of methyl /3-naphthyl ketone. 

Chemical Designations - Syrwnyms Palm butter Palm fruit oil Chemical Forrrmla Not applicable. Observable Cbaracteristics - Physical State (as shipped) Semi-solid to liquid Color Orange-red Odor Pleasant, characteristic. 

P-Acetoxy-5-hydroxy-B-mrcholestan-6-carboxylic Acid 5,6-Lactone (TO)."" A solution of 5 g (0.011 mole) of keto acid (69), 4.4 g of benzoyl chloride and 10 ml of anhydrous pyridine is allowed to stand for 3 days at room temperature. After a short period the mixture turns red-brown and at the end of the reaction the dark semi-solid mass is poured into 200 ml of water and extracted with two 100 ml portions of ether. The ethereal extracts are washed twice with equal portions of 5 % sodium hydroxide and water, dried and the ether evaporated. The red sirupy residue is mixed with 10 ml of methanol and a brown solid separates immediately. After standing for 1 hr the solid is removed by filtration and washed with methanol. A second crop is obtained upon concentration of the filtrate. The combined crops are recrystallized twice from methanol to give (70) as white needles mp 124-125° yield 2.8 g (58 %). 

It the oil contain more than a certain quantity of the latter body it ie semi-solid at ordinary temperatures, whilst in auy ease crystals are deposited oci exposure to oold. German oil is rich iu apiul, but French oil contains very little, Apiol is prepared trum the oil either as a thick liquid, or in the purer e.rvstalline condition, aud is used to some e-tleol in medicine. 

The fresh flowers of the mignonette, Heicda odoratu, yield traces, about -002 per oeut., of an essential oil of eieecdingiy powerful odour. This oil is semi-solid at ordinary temperatures, and its cberaistnr is not uoderslood, as the oil is in itself so very rare. Indeed, commercially, -an ordinary floral extract is generally used in preferenoe to any direct... 

An absolutely scientific definition of the term essential cr volatile oils is hardly possible, but for all practical purposes they may be defined as odoriferous bodies of an oily nature obtained almost exclusively from vegetable sources, generally liquid (sometimes semi-solid or solid) at ordinary temperatures, and volatile without decomposition. This definition must be accepted within the ordinary limitations which are laid down by the common acceptation of the words, which will make themselves apparent in the sequel, and show that no more restricted definition is either advantageous or possible. Many essential oils, for example, are partially decomposed when distilled by themselves, and some even when steam distilled. 

The crude ester is cooled, an equal volume of benzene is added, then the free acid is neutralized by shaking with about 250 cc. of a 10 per cent solution of sodium carbonate (Note 4). The benzene solution is poured into 1300 cc. of a saturated solution of sodium bisulfite (about 60 g. of technical sodium bisulfite per 100 cc.), contained in a wide-neck bottle equipped with an efficient stirrer, and the mixture stirred for two and a half hours. The mixture soon warms up a little and becomes semi-solid. It is filtered through a 20-cm. Buchner funnel and carefully washed, first with 200 cc. of a saturated solution of sodium bisulfite, finally with two 150-cc. portions of benzene (Notes 5 and 6). The white pearly flakes of the sodium bisulfite addition product are transferred to a 3-I. round-bottom wide-neck flask equipped with a mechanical stirrer and containing 700 cc. of water, 175 cc. of concentrated sulfuric acid, and 500 cc. of benzene. The flask is heated on a steam bath under a hood, the temperature being kept at 55°, and the mixture is stirred for thirty minutes (Note 7). The solution is then poured into a separatory funnel, the benzene separated and the water layer extracted with a 200-cc. portion of benzene. The combined benzene solution is shaken with excess of 10 per cent sodium carbonate solution to remove free acid and sulfur dioxide (Note 8). The benzene is washed with a little water and then dried over anhydrous potassium carbonate (Note 9). The benzene is distilled at ordinary pressure over a free flame from a 500-cc. Claisen flask, the solution being added from a separatory funnel as fast as the benzene distils. It is advisable to distil the ester under reduced pressure although it can be done under ordinary pressure. The fraction distilling around n8°/5mm., 130710 mm., 138715 mm., 148725 mm., 155735 mm., or... 

The rate of evaporation is greatly accelerated by allowing a stream of air to blow across the surface of the hot liquid. It is advantageous for the evaporation to proceed as far as possible in order to remove most of the free hydrochloric acid, and no harm is done if it continues until the solution turns to a semi-solid mass of crystals. 

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