Collection yield

Anfall, m. amount formed or collected, yield attack fit stay, prop. 

Urea (118 g, 1.96 mols) was added to 192 g (0.98 mol) of 3-(3, 5 -dlmethylphenoxy)-1,2-propane-diol which had previously been heated to 150°C. The reaction mixture was then heated rapidly to 195° to 200°C and maintained at this temperature for 5 hours with constant stirring. The resulting mixture was partitioned between water and ethyl acetate and the ethyl acetate layer was dried over sodium sulfate and concentrated. The residue was distilled in vacuo and the fraction boiling at 220° to 225°C/1.5 mm was collected. Yield, 172 g (79%). The distillate was crystallized from dry ethyl acetate MP, 121.5° to 123°C. 

An ice-cold solution of diazepinone 5a (1.76 g, 8.8 mmol) in 10% aq K.OH (10 mL, 18 mmol) was treated dropwisc with a solution of dimethyl sulfate (1.4 mL, 11.2 mmol) in MeOH (2mL), whereupon a red solid was precipitated. H20 (10mL) was added and the solid was filtered off, washed with 10% aq MeOH and suspended in MeOH (10 mL). 2M HC1 (15 mL) was added slowly, whereupon the solid dissolved and presently orange crystals of l,5-dimethyl-4-phenyl-l//-1,2-diazepin-6(7//)-one (12) appeared. H20 (10mL) was added and the product was collected yield 0.74g (39%) mp 71-72 C. The filtrate was made alkaline by slowly adding 40% K.OH, whereupon the betaine 13 separated yield 0.76 g (41 %) red plates mp 90-91 C (Et20). 

A mixture of betaine 13 (0.28 g, 1.3 mmol) and MeOH (2 mL) was warmed on a steam bath until the red color of the solution had faded to pale yellow (10-15 min). The solution was cooled and diluted with a small amount of H20 and the precipitated product, 1,5-dimethyl-6-phenyl-l H-, 2-diazcpin-4(7//)-one (14), was collected yield 0.22g (79%) mp 73-75 C (Et20/pentane). 

A 1-1. steel bomb is charged with 200 g. (1.51 moles) of dicyclo-pentadiene (Note 1). The bomb is flushed with ethylene (Note 2) and then filled while shaking to an initial pressure of 800-900 p.s.i. at 25°. Shaking is continued as the bomb is slowly heated (Note 3) to 190-200° and maintained at this temperature for 7 hours (Note 4). At the end of this period, the reaction vessel is cooled and vented, and the crude product is transferred into a simple distillation apparatus (Note 5). A fraction boiling between 93° and 100° is collected, yield 162-202 g. (57-71%, based on dicyclopentadiene) (Note 6). The norbornylene may be redistilled with negligible losses to give a final product, b.p. 94-97°/740 mm., m.p. 44-44.5° (sealed capillary). 

In Catalysis, navigating through a collection yields a like collection Bag->Bag, Sequence->Sequence, and so on. The asSet, asSeq, and asBag operators (or asType (T) equivalents) provide conversions. Thus, the following yields a bag of last names containing as many (possibly duplicated) entries as joe has friends. 

Several refinements of our experiments could test these theories further. By measuring etch pit densities as well as pit dimensions on sequentially-etched crystals, nucleation rate data and pit growth data could be collected, yielding information about the rate-limiting steps and mechanisms of dissolution. In addition, since the critical concentration is extremely dependent on surface energy of the crystal-water interface (Equation 4), careful measurement of Ccrit yields a precise measurement of Y. Our data indicates an interfacial energy of 280 + 90 mjm- for Arkansas quartz at 300°C, which compares well with Parks value of 360 mJm for 25°C (10). Similar experiments on other minerals could provide essential surface energy data. 

Method A The N-benzylimine (10 mmol), the acrylonitrile (10 mmol), and TEBA-C1 (10.2 g, 0.5 mmol) in DMSO or CH2C12 (5 ml) are stirred with aqueous NaOH (50%, 3 ml) for 30 min and then allowed to stand overnight. H20 (100 ml) is added and the precipitated pyrrolidine is collected [ yields are higher (60-80%) in DMSO]. 

S. Basu, B. Ellinger, S. Rizzo, C.l. Deraeve, M. Schurmann, H. Preut, H.-D. Arndt, and H. Waldmann, Biology-oriented synthesis of a natural-product inspired oxepane. Collection yields a small-molecule activator of the Wnt-pathway, Proc. Natl. Acad. Sci. USA., 108 (2011) 6805-6810. 

D-Threose diacetamide. (Aqua ammonia.) Thirty grams of tetraacetyl-o-xylononitrile was mixed with 300 ml. of concentrated aqua ammonia (28-29 %) and warmed on a water bath until the solid was all dissolved, and then allowed to stand for three hours. The solution was concentrated in vacuo to a thick sirup, which was dissolved in aqua ammonia and reconcentrated. The final thick sirup was dissolved in absolute ethanol and ether added to the point of turbidity. After forty-eight hours in a refrigerator the crystals which had formed were collected yield, 16.5 g. (78%). They were recrystallized by dissolution in two volumes of warm 75 % ethanol, filtration through carbon and the addition of an equal volume of absolute ethanol. The compound crystallized slowly, forming clear, sharp needles or prisms in resets, m. p. 165-167. ... 

Degradation of pentapropionyl-D-glucononitrile. (Sodium methoxide.Y - Five grams of pentapropionyl-n-glucononitrile was dissolved in 7 ml. of chloroform cooled to —6° and then a cool solution of 0.84 g. of sodium in 10 ml. of methanol was added. A jelly-like mass was produced that was kept in the ice-salt bath for five minutes. Fourteen milliliters of water and 2.5 ml. of acetic acid were then added. The water phase was separated and evaporated in vacuo 20 ml. of ethanol was added and the solvent evaporated again the operation was repeated once more. The final residue was dissolved in 26 ml. of water, and to 13 ml. 1 g. of diphenylhydrazine was added the solution was then heated in a water bath. When crystals of n-arabinose diphenyl-hydrazone appeared, heating was stopped, and after four hours in the cold the crystals were collected yield 54% (calcd. as n-arabinose), m. p. 204-205°. 

Fig. 9.4.8 Apparatus for the gas flow-cold trap method. One of the gas inlets is abbreviated in the figure. A cover in the figure is used to improve a collection yield. Without this, the particles produced just above a crucible are drifting in the chamber to deposit on the chamber wall. The end of the gas line is evacuated by a rotary pump so as to constantly flow the carrier gas. A solvent feeder is inserted on the gas line for the sublimation of organic liquid to deposit at the trapping apparatus cooled with liquid nitrogen. (From Ref. 10.)...

Purification of the crude material is accomplished by dissolving it in petroleum ether (30-50°) or methylene chloride, shaking this solution three times with water, and passing the organic layer through a fluted filter paper After the filtrate has been dried over anhydrous sodium sulfate, it is concentrated to a small volume and cooled to —78°. The perfectly white, crystalline product which separates is collected yielding 110-120 g. (30-33%) of crystals, m.p. 57-58° (Note 4). 

Two-thirds of resin 18 was treated with the Fmoc-Glu-S(CH2)2C02Et (19) y-HOBt ester (0.5 mmol). The resulting resin (1.4g) was treated with anisole/HF (1 9) at 0°C for 90min to give the crude product 20 (Xaa = Ahx 640 mg). This peptide was applied to a RP-HPLC column (20 mg at a time) and the main fraction collected yield (Xaa = Ahx) HOmg (12%). 

To the cooled (20-30°) mixture is added 240 g. of sodium chloride (Note 6). The resulting mixture is extracted with three 500-ml. portions of methylene chloride. The combined organic extracts are first washed with 40 ml. of 5% aqueous sodium bicarbonate solution (Note 7), and then with 300 ml. of saturated aqueous salt solution, dried over anhydrous sodium sulfate, and the solvent is distilled under reduced pressure (35 mm.) on a water bath (60-70°). The resulting residue weighing approximately 125 g. is fractionated under reduced pressure, and the fraction boiling at 100-103° (0.8 mm.) is collected yield 104 g. (76%) (Notes 8 and 9). 

In a 250-ml. three-necked flask equipped with a reflux condenser and a gas-inlet tube are placed 45,6 g. (0.4 mole) of 2-chloropyrimidine 2 and 150 ml. of absolute ethanol. The mixture is refluxed for 6 hours while anhydrous dimethylamine is bubbled into the solution (Note 1). The solution is cooled, and 100 ml. of ethanol is removed by distillation using a water aspirator. The residue is chilled in an ice bath for 1 hour, and 75 ml. of ether is added to cause precipitation of dimethylamine hydrochloride. After the removal of dimethylamine hydrochloride and solvent, the residue is distilled at reduced pressure from a Claisen flask (Note 2). The fraction boiling at 85 86°/28 mm. is collected yield 40 42.5 g. (81 86 ,), 1.5420 (Note 3). 

Cu(C104)2 6H20 (22.2mg, 0.06mmol) was reduced with copper wire under ethylene in methanol (10 mL). After the replacement of ethylene to argon atmosphere, the resultant Cu(I) solution was added to the L (18.2mg, 0.18mmol). The colorless solution was sealed in a 7-mm glass tube and allowed to stand at room temperature for a week. Colorless plate crystals were collected. Yield 16mg (20%). 

Bis[triisopropylgennyl] Tellurium4 Into a nitrogen-flushed ampoule are placed 0.67 g (5.3 mmol) of finely powdered tellurium, 15 ml of tetrahydrofuran, and 3.2 g (5.3 mmol) of bis[triisopropylgermyl] mercury. The ampoule is scaled, shaken at 70° for 30 h, cooled, and then carefully opened. The solution is decanted from mercury, the solvent is removed under reduced pressure, the residue is dissolved in the minimum amount of hexane, the solution is cooled to — 78°, and the crystals are collected yield 2.2 g (78%) m.p. 23°. 

Tetrakis[thiourea]tellurium Dithiocyanate6 3.0 g (7.6 mmol) of bis[thiourea]tellurium dithiocyanate are dissolved in 75 ml of 10% aqueous thiourea solution at 40°. The solution is filtered, the filtrate is kept at 20° overnight, and the deposited crystals are collected yield 3.4 g (72%). 

Tellurium Tris[dicthyldithiocarbamate] Chloride1 At 20° a solution of 0.67 g (2.5 mmol) of tellurium tetrachloride in 100 ml of ethanol is added dropwise to a solution of 1.3 g of sodium diethyldithiocarbamate trihydrate in 50 ml of ethanol. The mixture is allowed to stand overnight and is then heated to 50°. The warm mixture is filtered, the filtrate is covered with a layer of petroleum ether, and the crystals, which are formed after a few days, are collected yield 1.1 g (73%) m.p. 136° (ethanol). 

Trimethylsilylamino Tellurium Pentafluoride 16.1 g (0.1 mol) of bis[trimethylsilyl]amine are placed in a 250 ml stainless steel vessel which is then cooled to —196°. 31.4 g (0.13 mol) of tellurium hexafluoride are condensed into the vessel which is then sealed, warmed to 20°, and stirred at this temperature for 12 h. The resultant mixture is distilled in a glass apparatus and the fraction boiling at 58°/12 torr is collected yield 31 g (100%) m.p. 9° b.p. 58°/12 torr. 

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