Residue yields

Sulfur content and specific gravity as a function of residue yield. 

Rerunning operations are characterized by large volumes of distillate products and relatively small residue yields. Frequently, the product is withdrawn as a sidestream with undesirable light fractions passing overhead and polymers being withdrawn from the bottom of the tower. Lube rerun stills usually have several sidestreams which permit close control of flash point and viscosity while producing a wide range of stocks. 

A mixture of 5 g of the 21-acetate of SCt-chlorohydrocortisone, 7 g of chloranii and 100 cc of n-amyl alcohol was refluxed for 16 hours, cooled and diluted with ether. The solution was successively washed with water, 5% sodium carbonate solution and water, dried over anhydrous sodium sulfate, filtered and evaporated to dryness under reduced pressure. Chromatographic purification of the residue yielded the 21-acetate of 6-chloro-A -pregnatriene-11 3,17a,21 -triol-3,20-dione. ... 

A mixture of 0.1 mol of N-mono-1-p-chlorobenzohydrylpiperazine and 0.1 mol of 1-chloro-2-(2-hydroxy-ethoxy)-ethane is heated for 3 hours to 150°C. The mass is then taken up in 100 ml of benzene and 100 ml of a 10% aqueous solution of NaOH decanting takes place, and the benzene solution is washed with water and the solvent is evaporated. Vacuum distilling of the residue yields 1-p-chlorobenzohydryl-4-[2-(2-hydroxy-ethoxy)-ethyl]-piperazine, BP 220 C/0.5 mm Hg. 

A solution of 4.62 grams of 2-phenylcyclopropanecarboxylic acid in 15 cc of dry benzene is refluxed with 4 cc of thionyl chloride for 5 hours, the volatile liquids are removed and the residue once more distilled with benzene. Fractionation of the residue yields the carbonyl chloride of 2-phenylcyclopropane. 

A solution of 10-(piperazin-l-yl)-10,ll-dihydrodibenzo[6,/]thiepin (2.5 g, 8.4 mmol) in 100% formic acid (20 mL) was refluxed at 150 C for 6 h. The excess acid was removed by distillation at reduced pressure and the residue was treated with 10% aq NH3 (20mL), extracted with benzene (50mL) and the benzene solution was washed with dil HC1 and evaporated to dryness to give a neutral residue yield 1.8 g (98 %) mp 88 C (EtOH) (Note benzene should be replaced by organic solvents with lower toxicity). 

Tetra-ter/-butyl-1,4,8,ll,15,18,22,25-octaazaphthalocyanine (0.1 g) was dissolved in CHC13 (400 mL), CoCl2 in EtOH (sat. by boiling, 150 mL) was added, and the mixture was refluxed for 2 min. The solvent was evaporated under vacuum and extraction with CHC13 from the residue yielded the title compound. It was purified by column chromatography. The impurities were eluted with CHCI, and the dye 3 was eluted with benzene/acetone (2 1) yield 0.072 g 12%). 

The 42 per cent hydrazine hydrate solution supplied by the Eastman Kodak Company is too dilute for use as such, but may be concentrated by distillation with xylene.1 A mixture of r44 cc. (150 g.) of the 42 per cent solution and 230 cc. of xylene is distilled from a 500-cc. flask through a 17-cm. Hempel column fitted into a cork covered with tin foil. After distillation of the xylene, with about 85 cc. of water, the residue yields on distillation 45-50 g. of 80-85 per cent hydrazine hydrate. This material, assayed best by titration with standard acid using methyl orange as indicator, may be used as such or concentrated further (see Note 6). 

In contrast, when a THF-acetonitrile solution of [26+jClOj or [113+JC104 was added to the THF solution of K+[2 ], the deep green colour of carbanion [2 ] persisted. After evaporation of the solvent, purification of the residue yielded a dark green salt, [26+2 ] or [113+2 ] (Scheme 3), the IR spectra (KBr disk) of which consisted of the absorptions of [2 ] and [26+] or [113+] superimposed. The visible-near IR region... 

Both 1st- and 2nd-order rate expressions gave statistically good fits for the control samples, while the treated samples were statistically best analyzed by 2nd-order kinetics. The rate constants, lst-order activation parameters, and char/residue yields for the untreated samples were related to cellulose crystallinity. In addition, AS+ values for the control samples suggested that the pyrolytic reaction proceeds through an ordered transition state. The mass loss rates and activation parameters for the phosphoric acid-treated samples implied that the mass loss mechanism was different from that for the control untreated samples. The higher rates of mass loss and... 

The ether is distilled through a small column (Note 6), under reduced pressure, from a 1-1. flask which is heated by a bath whose temperature is gradually raised to about 60°. The residual yellow liquid is transferred, with the aid of a little anhydrous ether, to a 100-ml. flask, and the remaining solvent is distilled through the column under reduced pressure. Rectification of the residue yields 2-3 g. of fore-... 

One category comprises products of oxidized lysine or hydroxylysine amino acid residues with another lysine or hydroxylysine residue yielding difunctional cross-links. These cross-links may then react with another... 

These conformer populations were confirmed by a number of n.O.e. measurements (the H2—H5 distance can act as a marker in identifying the ring form). The case of a hexasaccharide (compound 23 in Ref. 9) where the three IdoA residues yield different n.O.e. enhancements, is striking. Moreover, models computed with molecular mechanics have been put forward for the peculiar pentasaccharide of heparin. The models are in acceptable agreement with the observed vicinal coupling constants and n.O.e. values (10) (a full paper by Ragazzi, M. et al. Carbohvdr. Res.. is in press). 

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