Light filter neutral

A mixture of the arylsulfonyl chloride (5 mmol), benzene (2.56 mol), NaN3 (5 mmol), NaHCO, (20 mmol), and methyltrioctylammonium chloride (0.5 mmol), under N2 in an autoclave, was stirred al 40 C for 3 h. The mixture was then heated slowly to 125 C and maintained at this temperature for another 3 h, during which time the pressure in the vessel rose to 31 -54 atm. The mixture was allowed to cool and the autoclave was depressurized. The residual mass was filtered, and the residue washed thoroughly with cold H20. The benzene solution was separated from the aqueous filtrate, dried, and evaporated to give the crude product as a reddish yellow mass which was purified by column chromatography (neutral alumina, hexane/ benzene 3 2). The 1-(arylsulfonyl)-l//-azepines 16 were crystallized from light petroleum ether (bp 60-80 LC). 

In one method the intensity of the primary beam is diminished by several orders of magnitude through the use of a series of neutral filters, the percentage transmission of each at the wavelength X having been accurately measured. Comparison of the intensity of light scattered by the solution with the intensity of the incident beam meas-... 

Turanose Phenylosotriazole. A solution of 15 g. of turanose phenylosazone in 300 cc. of hot water was placed on the steam-bath and a solution of 22 g. of copper siilfate pentahydrate in 150 cc. of hot water was added. The mixture turned a deep cherry-red at once and in a short time (fifteen min.) a red precipitate had formed and the solution had become green. After thirty minutes from the time of addition of the copper solution, the solution was cooled, filtered, and the copper removed as sulfide. The clear light yellow filtrate was neutralized with 45 g. of barium carbonate and the insoluble material removed by filtration. The filtrate was extracted with five 50-cc. portions of ether to remove the aniline, and the aqueous portion was concentrated in vacuo to a thick sirup. The sirup was dissolved in 60 cc. of warm alcohol, filtered to remove a slight turbidity and diluted with 65 cc. of ether. Upon cooling and scratching, the product crystallized as large prisms yield 8.9 g. (72%). The phenylosotriazole was recrystallized from 10 parts of alcohol and when pure showed the melting point 193-194° and rotated [a Jj" + 74.5° in aqueous solution (c, 0.90). 

In dim red light, the weighed hydrazide contained in one of the 500 ml flasks (ca. 67 g 95% of theory) is washed into a 1000 ml beaker with 263 ml IN hydrochloric acid. 239 ml distilled water, 239 ml ethanol (95%), and 37 ml 2,4-pentanedione are added, and the well-mixed solution left to stand in the dark at room temperature until the reaction is complete, i.e., about 30 minutes. The reaction mixture is neutralized with the addition of 263 ml 1 N sodium hydroxide, and the beaker covered with parafilm and refrigerated to ensure complete precipitation. The pyrazole is filtered at the pump, the mother liquor being returned to the beaker and used to wash out the last few crystals, washed with cold water, and sucked dry under a stream of dry nitrogen. The product is dried in vacuo over barium oxide or phosphorus pentoxide for at least twelve hours before proceeding to the next step, wherein anhydrous conditions will increase yield. Hofmann calls for drying the pyrazole in vacuo at 60°, which indicated the product to be fairly stable. So all the hydrazide is converted prior to aminization. 

The initiation system consists of a nitrogen laser and the necessary optics to lead the beam to the sample cell. The laser emits pulses at 337.1 nm with 800 ps duration, with a typical repetition rate of less than 5 Hz. The optical components, aligned between the laser and the calorimetric cell, consist of an iris (I), a support for neutral density filters (F), and a collimating lens (L). The iris is used to cut out most of the laser output and allow only a thin cylinder of light to pass through its aperture, set to 2 mm. The laser energy that reaches the cell is further... 

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