Butane residual atmosphere

The characteristic times for waste destmction to an efficiency of 99.99%, for water in a nitrogen atmosphere, where the residue is a typical hydrocarbon breaking into two large fragments, eg, / -butane decomposing into two ethyl radicals would be droplet heatup, 0.073 s droplet evaporation,... 

Dichlorobutane. Place 22.5 g (0.25 mol) of redistilled butane- 1,4-diol and 3 ml of dry pyridine in the flask in an ice bath. Add 119 g (73 ml, 1 mol) of redistilled thionyl chloride dropwise to the vigorously stirred mixture at such a rate that the temperature remains at 5-10 °C. When the addition is complete, remove the ice bath, keep the mixture overnight and then reflux for 3 hours. Cool, add ice-water cautiously and extract with ether. Wash the ethereal extract successively with 10 per cent sodium hydrogen carbonate solution and water, and dry with magnesium sulphate. Remove the ether by flash distillation and distil the residue under reduced pressure. Collect the 1,4-dichlorobutane at 55.5-56.5 °C/14mmHg the yield is 18 g (58%). The b.p. under atmospheric pressure is 154-155 °C. 

A solution of 3-(4-chloro-5-fluoropyrimidin-6-yl)-2-(2,4-difluorophenyl)-l-(lH-l,2,4-triazol-l-yl)butan-2-ol, enantiomeric pair B (0.307 g, 0.8 mmol) in ethanol (20 ml) was hydrogenated at atmospheric pressure and at room temperature in the presence of 10% palladium-on-charcoal (30 mg) and sodium acetate (0.082 g, 1 mmol). After 5 hours a further 10 mg of 10% palladium-on-charcoal was added and hydrogenation was continued for an additional 1 hour. The catalyst was removed by filtration and the filtrate was concentrated in vacuo. Flash chromatography of the residue on silica using 97 3 ethyl acetate/methanol as the eluent provided, after combination and evaporation of appropriate fractions and trituration with diethyl ether, the 2-(2,4-difluorophenyI)-3-(5-fluoropyrimidin-4-yl)-l-(lH-l,2,4-triazol-I-yl)butan-2-ol enantiomeric pair B, (0.249 g, 89%), m.p. 127°C. 

Tetraethyl butane-1,1,4,4-tetrtacarboxylate added to a soln. of Na in abs. alcohol, to the resulting soln. tetraethyl l,4-dibromobutane-l,l,4,4-tetracarboxy-late added, and heated 4 hrs. in an oil bath at no-IIS -> tetraethyl cyclobutane-1,1,2,2-tetracarboxylate (Y 75.2%) boiled with aq. HGl (1 1) at ISO-HO in an oil bath until the oily layer has dissolved after 35-40 hrs., the HGl removed by distillation, and the residue heated at 180-200° until G0.2-evolution ceases mixture of cis- and frans-cyclobutane-l,2-dicarboxylic acids (Y 97.5%) refluxed 5 hrs. at 70-90° with acetjd chloride on a water bath, excess acetyl chloride and the resulting acetic acid removed by distillation at atmospheric pressure, and the residue heated 6-7 hrs. at 160-175° in an oil bath whereby the mixed anhydride of frans-cyclobutane-l,2-dicarboxylic acid and acetic acid is converted to acetic anhydride and cis-cyclobutane-l,2-dicarboxylic acid anhydride (Y 81.2%) boiled with 2 parts of water cis-cyclobutane-l,2-di-carboxylic acid (Y ca. 100%). V. P. Gol mov and Z. P. Malevannya, 7K. 31, 665 (1961) G. A. 55, 22162b method of ring closure s. J. J. Lennon and W. H. Perkin, Soc. 1928, 1513. 

Characterization of Mixed-Gas Permeation Properties. The mixed-gas permeation properties of isotropic PMP films were determined for several /i-butane/methane mixtures. The permeation experiments were performed using the constant pressure/variable volume method (8) at a feed pressure of 150 psig and atmospheric permeate pressure (0 psig). The feed temperature was varied between 0 C and 50°C. The following -butane/methane feed mixtures were used 1, 2, 4, 6, and 8 mol% w-C4H10 in CH4, respectively. The stage-cut, that is, the permeate flow rate to feed flow rate was less than 1%. Thus, the residue composition was essentially equal to the feed composition. The feed, residue, and permeate compositions were determined with a gas chromatograph equipped with a thermal conductivity detector. 

---