Reference of 2163-00-0, The chemical industry reduces the impact on the environment during synthesis 2163-00-0, name is 1,6-Dichlorohexane, I believe this compound will play a more active role in future production and life.
Example 4; A nitrogen-purged stirred 2 l four-necked flask apparatus with internal thermometer, reflux condenser with bubble counter and pH electrode was initially charged with 136.5 g (0.55 mol) of sodium thiosulphate pentahydrate and 300 g of deionized water. The stirrer was switched on. After the thiosulphate had dissolved, 38.8 g (0.25 mol) of 1,6-dichlorohexane were added. The weakly acidic mixture was adjusted to pH 7.2+/-0.1 with 2.5% sodium hydroxide solution. The reaction vessel was purged once again briefly with nitrogen and the mixture was then boiled at reflux for 9 h, and the pH of the reaction mixture was kept at 7.2+/-0.1 during this time by addition of 2.5% sodium hydroxide solution by means of a metering pump (control by means of pH electrode). After in each case 6 and 8 hours of the reaction, the bubble counter was removed briefly from the reflux condenser. In each case approx. 5 ml of demineralized water were then sprayed with a wash bottle into the reflux condenser from the top in order to flush back into the flask any 1,6-dichlorohexane which has not dripped back. After the reaction time had ended, approx. 15 ml of 2.5% sodium hydroxide solution were used for pH control. After brief cooling, a small sample was taken from the reaction mixture to determine the conversion of 1,6-dichlorohexane by gas chromatography (GC). The GC analysis with internal standard gave a residual content of 1,6-dichlorohexane <10 ppm, which corresponds to a conversion of 1,6-dichlorohexane of >99.9%. The reaction mixture cooled to room temperature was admixed with 21.0 g (0.25 mol) of aqueous formaldehyde solution (36-38%), 21.0 g (0.25 mol) of sodium hydrogencarbonate and 43.3 g of toluene (25 parts by weight based on 100 parts by weight of the theoretically expected yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane). The headspace of the reactor was purged once again briefly with nitrogen. As soon as the hydrogencarbonate had dissolved, the feed of 773.3 g (0.5 mol) of sodium dibenzyldithiocarbamate solution (NaBEC solution) (19.1%) which had a temperature of approx. 22 C. was commenced at an internal reactor temperature of approx. 23 C. During the uniform feeding of the NaBEC solution over 1 h, the internal reactor temperature was kept at approx. 23 C. On completion of feeding, the mixture was stirred at approx. 23 C. for a further 22 h. Immediately before the commencement of the NaBEC feeding, the pH was approx. 8.3. On commencement of the NaBEC feeding, the pH rose very sharply and attained a value of approx. 10.7 at the end of the NaBEC feeding. At the end of the continued stirring time, the pH was likewise approx. 10.7. It was possible to isolate the precipitated solid very readily by suction filtration. The product was washed on the suction filter with a total of 2 1 of demineralized water in portions, which proceeded very easily. The product was dried at 50 C. and approx. 150 mbar in a vacuum drying cabinet to constant weight. The yield was approx. 91% of theory based on 1,6-dichiorohexane used. The content of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was determined to be approx. 96% by means of HPLC (external standard). The melting point was approx. 92 C. The ignition residue (750 C./2 h) of the product was approx. 0.2% by weight.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1,6-Dichlorohexane, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Buding, Hartmuth; Weidenhaupt, Hermann-Josef; Jeske, Winfried; Kleiner, Thomas; US2005/272933; (2005); A1;,
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