Residue dried

The use of a ternary mixture in the drying of a liquid (ethyl alcohol) has been described in Section 1,5 the following is an example of its application to the drying of a solid. Laevulose (fructose) is dissolved in warm absolute ethyl alcohol, benzene is added, and the mixture is fractionated. A ternary mixture, alcohol-benzene-water, b.p. 64°, distils first, and then the binary mixture, benzene-alcohol, b.p. 68-3°. The residual, dry alcoholic solution is partially distilled and the concentrated solution is allowed to crystallise the anhydrous sugar separates. 

The hydrogen sulfate was dissolved in water and the pH of the solution was adjusted to 5.6 (pH-meter) with 0.1 N sodium hydroxide solution. The water solution was evaporated to dryness and the residue dried with absolute ethanol/benzene and once more evaporated to dryness. The remaining crystal mixture was extracted in a Soxhiet extraction apparatus with absolute methanol. From the methanol phase the sulfate of 1-(3, 5 -dihydroxyphenyl)-2-(t-butylaminoj-ethanol crystallized. Melting point 246°C to 248°C. 

The mixture was then hydrogenated at just above atmospheric pressure for 1 A hours and filtered through a Dicalite bed. The clear filtrate was evaporated at low temperature and pressure, and the residue dried in vacuo over phosphorus pentoxide, to give 1.64 g of the salt of Q-(3-thienyl)methylpenici lin as a white solid. 

Benzazepin-2-amine (3 20 g, 0.126 mol) was added cautiously to 90% HN03 (100 mL) at 0 C. The acidic solution was stirred at 0-10 C for ca. 3 h and then at 10 C for a further 2 h. The solution was poured onto ice and the precipitate collected by filtration. The precipitate after being washed with acetone was slurried with H20 and then neutralized with sat. aq Na2C03. The mixture was filtered, and the residue dried to give the product as an orange solid yield 20 g (84%) mp 200-203 C. 

CHCI3. The organic layer was evaporated to dryness and the residue dried at 105 C for 3 hours. Chlorpromazine was weighed as its brominated derivative. 

The light brown color turns to red whereupon the temperature is permitted to rise to — 78 °C within 30 min. Excess boron trifluoride is permitted to evaporate and escape through the exit valve. The cap with the glass tube is removed and the Schlenk tube is stoppered. Residual boron trifluoride is removed in vacuo at — 60 °C for 1 h. The product is precipitated at — 60 °C with 80 mL of cold diethyl ether. The solvent is decanted and the red residue dried in vacuo at or below — 50 °C for 1 h. At this temperature, it is reprecipitated from dichloromethane (40 mL) with diethyl ether (80 mL) precooled to — 50 °C. After removal of the solvent as above, 3.5 g (71%) of the title compound is obtained. 

Method 3(when acardite II centralites are present) a)Extract with chlf or methylene chloride ca lOg of finely divided propellant, evap the solvent and weigh the dried extract (wt 1 - centralite + acardite II) b)Treat the extracted material with aq AcOH at pH ca 4 and filter the mixt through cared sintered glass crucible. Rinse the residue, dry it to const wt and weigh(wt 2 = acardite II and wt 1 — wt 2 centralites) c)Continue. the analysis as described in procedures (c) to (g) of Method 4... 

Peuckner adopts a somewhat modified process. Sulphide of sodium is prepared by igniting sulphate of soda with charcoal powder. This is dissolved In water, some free sulphur is added, the liquid Is concentrated, mixed With one half per cent, of sulphate of iron and twenty-five per cent, of a well-tempered day—the purer and whitar the better—the mixture evaporated to dryness, the residue powdered, and ignited for an hour in a cupelling furnace when cold, it is extracted with water, the residue dried, powdered, and once more heated in a muffle, when the required tint appears. 

Substances Insoluble in Acetic Acid. — To 2 gm. of lead oxide mixed with 5 cc. of water add 10 cc. of dilute acetic acid. No evolution of gas should take place. Now boil the liquid for several minutes, filter when cold, wash the undissolved residue, dry at 100° C., and weigh. The weight should not exceed 0.005 gm. 

Iron and Potassium. — Decompose 10 gm. of sodium oxalate by igniting moderately in a platinum crucible, removing the last traces of carbon by cautious ignition with a blast lamp. The residue, when treated with warm water in a platinum dish, should be completely soluble, and should leave at most a scarcely weighable trace of undissolved iron oxide. The solution is filtered if necessary, and supersaturated with hydrochloric acid as free from iron as possible. It is then evaporated in a platinum dish on the water-bath, and the residue dried for two hours in the drying oven at 120° C. The residue must dissolve clear in water and the solution should give ... 

The crude TFA salt 12 was dissolved in CHC13 (1.0 M) and cooled to 0°C. TEA (5 equiv) and a soln of the crude acid 11 in DMF (1.0 M) were added successively. Subsequently, HOBt (1.2 equiv) and EDC (1.2 equiv) were added portionwise. The mixture was allowed to warm to rt and stirring was continued for 16 h. The mixture was concentrated and the residue dried under high vacuum. Stirring the resulting residue in MeOH for 20 min resulted in a white precipitate that was collected by filtration and washed successively with MeOH and MeOH/H20 (1 1) yield 480mg (72%). The product 8 was dried under high vacuum over KOH mp 240 °C (dec) [a]Drt —34.6 (c 1, TFE). 

The amino diester 34 (30.5 g, 52.5 mmol) was dissolved in dioxane (130 mL) and the resulting soln was treated with 1 M NaOH (63 mL) at rt for 4h. The mixture was then treated with 3 M HC1 (63 mL) and concentrated under reduced pressure. The residue was taken up in toluene and re-concentrated (3 x) and the residue dried in vacuo. The resulting a-amino ester monoacid was dissolved in dry DMF (1800mL), cooled to 0°C, and treated sequentially with TEA (22 mL, 157.5 mmol) and DPPA (22.6 mL, 105 mmol). The mixture was brought to rt and stirred for 48 h. The mixture was concentrated under reduced pressure and the residue purified by flash chromatography (silica gel, 10 x 24 cm column, 15-20% EtOAc/hexane) to give 35, contaminated with the saturated a-amino ester yield 19.83 g (69%). 

To a soln of cyclic template c[-Amhn-Lys-Gly-Lys-Pro-Gly-Lys-Gly-Lys-] -4 HC1 (see Section 13.1.1.1.2) (10 mg, 9 pmol) in DMF (2mL) (at 0°C), DIPEA (7 pL, 39.5 pmol) and (Et0)2CHC02Su (19 mg, 39.5 pmol) were added slowly and the mixture stirred at rt for 3 h. The solvent was removed and the residue redissolved in EtOAc (10 mL). The organic phase was washed with 10% citric acid (3 x), H20 (1 x), and dried (Na2S04). EtOAc was removed and the residue dried in high vacuo yield 7.7mg (56%). The residue was treated with H20/1.2M HC1 (1 1) in order to hydrolyze the tetrakis(diethyl acetal). After 1 h stirring at rt, the solvent was removed in high vacuo. This procedure was repeated three times as the completion of hydrolysis was monitored by analytical HPLC. The residue was purified by HPLC and lyophilized yield 3 mg (66%). 

In a mortar containing a considerable amount of calcined coarse sand or pumice are placed 3-5 grams of the cheese, the whole being maintained for some hours in an oven at about ioo°, or better in a vacuum over sulphuric acid. The cheese is then well pounded with the sand and the mixture placed in a paper thimble and extracted with anhydrous ether in an extraction apparatus for 4 hours. The residue is subsequently pounded again and extracted anew for 2 hours with fresh ether. The united ethereal solutions are distilled and the residue dried for an hour at 100 0 and weighed. 

---