Category: 2163-00-0

Synthetic Route of 2163-00-0, These common heterocyclic compound, 2163-00-0, name is 1,6-Dichlorohexane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Examples 2 to 5; The procedure of Example 1 was repeated, except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9. Before the start of the particular reaction, the weakly acidic mixture was adjusted to the pH of 5, 6, 8 and 9 with 2.5% sodium hydroxide solution (measurement with pH electrodes). Example 2 Example 3 Example 4 Example 5 pH value in 5.0 +/- 0.1 6.0 +/- 0.1 8.0 +/- 0.1 9.0 +/- 0.1 the reaction Residual 1,6-dichloro- <10 <10 <10 approx. 11 hexane content (ppm) Conversion of 1,6- >99.9 >99.9 >99.9 >99.9 dichlorohexane (%) In all examples (Examples 2 to 5), the resulting reaction mixture was clear and homogeneous. To determine the pure yield with respect to Examples 2 and 5, they were repeated once more. However, a GC analysis sample was not taken from the particular reaction mixture. The pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate was approx. 91.4%2) for the repetition of Example 2 and approx. 90.6%2) for the repetition of Example 5. 2) The pure yield for the synthesis according to Examples 2 and 5 was carried out again as in Example 1 by reacting the reaction solutions obtained in each case with aqueous NaBEC solution. In this procedure, the yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was approx. 89.6% of theory with a content of 95% for the reaction according to Example 2 and approx. 89.7% of theory with a content of approx. 94% for that according to Example 5. Thus, the pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate in the inventive reaction of 1,6-dichlorohexane with sodium thiosulphate pentahydrate must have been approx. 91.4% for the reaction according to Example 2 (89.6%×0.95×1/0.931=91.4%) and approx. 90.6% for that according to Example 5 (89.7%×0.94×1/0.931=90.6%).

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Buding, Hartmuth; US2005/240044; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2163-00-0, name is 1,6-Dichlorohexane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 1,6-Dichlorohexane

A 250 mL four-necked flask equipped with a mechanical stirrer, a thermometer and a reflux condenser was used as the reaction vessel. 32. 3 g (0.13 mol) of sodium thiosulfate pentahydrate was weighed out, 70.0 g of water and 35. 0 g of DMF were added, After stirring and dissolving, 9.3 g (0.06 mol) of 1,6-dichlorohexane was added while stirring. The temperature of the solution was raised by heating, and the temperature of the reaction solution was raised to 90 C. The reaction was stirred at this temperature for 6 h, Hexamethylene-1,6-dithiosulfate disodium salt (HTS) solution. The resulting hexamethylene-1,6-dithio-sulfate disodium salt solution was analyzed by a gas chromatograph (GC) and a liquid chromatograph (HPLC), respectively, to measure 1,6-dichlorohexane and thiosulfate Sodium in the solution

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Red Avenue Innova Co., Ltd; Zhen, Boming; Dong, Dong; Zhao, Lili; fang, Caiqin; Ruan, zhen Gang; Hu, Xiaona; (10 pag.)CN105218419; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 2163-00-0, name is 1,6-Dichlorohexane, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H12Cl2

EXAMPLE 2A 1,6-Bis(4-cyanomethylmorpholinium)hexane Dichloride (HDMMA) 100 ml of morpholine (1.147 mole) and 150 ml ethylacetate (EtOAc) were added to 500 ml Morton flask equipped with reflux condenser, thermometer, mechanical stirrer, and heating mantel. 25 ml of 1,6-dichlorohexane (0.172 mole) was added slowly to flask at room temperature. This was refluxed for 48 hours. Gas chromatogram showed 90% completion of the reaction. The product 1,6-bismorpholinohexane was purified from reaction mixture by vacuum filtration to remove the morpholine hydrochloride, and the light yellow filtrate was purified by adsorption chromatography. 13 C NMR showed a spectrum consistent with structure with very minor impurities. Gas chromatography showed an approximate purity of 98.2% based upon peak areas. The collected amount of 1,6-bismorpholinehexane was 30.0 g, which corresponds to a yield of 66.6%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 2163-00-0.

Reference:
Patent; The Clorox Company; US5739327; (1998); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2163-00-0, name is 1,6-Dichlorohexane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 2163-00-0

Examples 2 to 5; The procedure of Example 1 was repeated, except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9. Before the start of the particular reaction, the weakly acidic mixture was adjusted to the pH of 5, 6, 8 and 9 with 2.5% sodium hydroxide solution (measurement with pH electrodes). Example 2 Example 3 Example 4 Example 5 pH value in 5.0 +/- 0.1 6.0 +/- 0.1 8.0 +/- 0.1 9.0 +/- 0.1 the reaction Residual 1,6-dichloro- <10 <10 <10 approx. 11 hexane content (ppm) Conversion of 1,6- >99.9 >99.9 >99.9 >99.9 dichlorohexane (%) In all examples (Examples 2 to 5), the resulting reaction mixture was clear and homogeneous. To determine the pure yield with respect to Examples 2 and 5, they were repeated once more. However, a GC analysis sample was not taken from the particular reaction mixture. The pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate was approx. 91.4%2) for the repetition of Example 2 and approx. 90.6%2) for the repetition of Example 5. 2) The pure yield for the synthesis according to Examples 2 and 5 was carried out again as in Example 1 by reacting the reaction solutions obtained in each case with aqueous NaBEC solution. In this procedure, the yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was approx. 89.6% of theory with a content of 95% for the reaction according to Example 2 and approx. 89.7% of theory with a content of approx. 94% for that according to Example 5. Thus, the pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate in the inventive reaction of 1,6-dichlorohexane with sodium thiosulphate pentahydrate must have been approx. 91.4% for the reaction according to Example 2 (89.6%×0.95×1/0.931=91.4%) and approx. 90.6% for that according to Example 5 (89.7%×0.94×1/0.931=90.6%).

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Buding, Hartmuth; US2005/240044; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2163-00-0, name is 1,6-Dichlorohexane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

A 250 mL four-necked flask equipped with a mechanical stirrer, a thermometer and a reflux condenser was used as the reaction vessel. 32. 3 g (0.13 mol) of sodium thiosulfate pentahydrate was weighed out, 70.0 g of water and 35. 0 g of DMF were added, After stirring and dissolving, 9.3 g (0.06 mol) of 1,6-dichlorohexane was added while stirring. The temperature of the solution was raised by heating, and the temperature of the reaction solution was raised to 90 C. The reaction was stirred at this temperature for 6 h, Hexamethylene-1,6-dithiosulfate disodium salt (HTS) solution. The resulting hexamethylene-1,6-dithio-sulfate disodium salt solution was analyzed by a gas chromatograph (GC) and a liquid chromatograph (HPLC), respectively, to measure 1,6-dichlorohexane and thiosulfate Sodium in the solution

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Red Avenue Innova Co., Ltd; Zhen, Boming; Dong, Dong; Zhao, Lili; fang, Caiqin; Ruan, zhen Gang; Hu, Xiaona; (10 pag.)CN105218419; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2163-00-0, These common heterocyclic compound, 2163-00-0, name is 1,6-Dichlorohexane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Examples 2 to 5; The procedure of Example 1 was repeated, except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9. Before the start of the particular reaction, the weakly acidic mixture was adjusted to the pH of 5, 6, 8 and 9 with 2.5% sodium hydroxide solution (measurement with pH electrodes). Example 2 Example 3 Example 4 Example 5 pH value in 5.0 +/- 0.1 6.0 +/- 0.1 8.0 +/- 0.1 9.0 +/- 0.1 the reaction Residual 1,6-dichloro- <10 <10 <10 approx. 11 hexane content (ppm) Conversion of 1,6- >99.9 >99.9 >99.9 >99.9 dichlorohexane (%) In all examples (Examples 2 to 5), the resulting reaction mixture was clear and homogeneous. To determine the pure yield with respect to Examples 2 and 5, they were repeated once more. However, a GC analysis sample was not taken from the particular reaction mixture. The pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate was approx. 91.4%2) for the repetition of Example 2 and approx. 90.6%2) for the repetition of Example 5. 2) The pure yield for the synthesis according to Examples 2 and 5 was carried out again as in Example 1 by reacting the reaction solutions obtained in each case with aqueous NaBEC solution. In this procedure, the yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was approx. 89.6% of theory with a content of 95% for the reaction according to Example 2 and approx. 89.7% of theory with a content of approx. 94% for that according to Example 5. Thus, the pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate in the inventive reaction of 1,6-dichlorohexane with sodium thiosulphate pentahydrate must have been approx. 91.4% for the reaction according to Example 2 (89.6%¡Á0.95¡Á1/0.931=91.4%) and approx. 90.6% for that according to Example 5 (89.7%¡Á0.94¡Á1/0.931=90.6%).

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Buding, Hartmuth; US2005/240044; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics