Category: 1070-64-0

These common heterocyclic compound, 1070-64-0, name is Ethyl 6,8-dichlorooctanoate, 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. name: Ethyl 6,8-dichlorooctanoate

1, 100 g (0.4mol) racemic Ethyl 6, 8-Dichlorooctanoic acid (95% industrial grade) is prepared first, and then treated with an alkali hydrolysis process so as to obtain (+/-)-DCA 80 g, to be dissolved into 300 ml ethyl acetate, followed by 24 g (0.2 mol) S-(-)-alpha-phenethylamine, afterwards, gradually cooled down to a temperature range between 0-10 C., overnight, filtered, and ultimately obtain 30 g wet (+)DCA S-(-)-alpha-phenethylamine salt. Afterwards, a recrystallization process is followed, wherein the (+)DCA-S-(-)-alpha-phenethylamine salt is dissolved in the ethyl acetate, and acidified with diluted hydrochloric acid, and extracted by methylbenzene, and distilled at low temperature to remove solvent, finally obtain 18.8 g (+)-DCA, [alpha]D25+48-49.6 with a yield rate from 42% to 46%.

The synthetic route of Ethyl 6,8-dichlorooctanoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nanjing Rally Biochemical Inc.; US2007/15926; (2007); A1;,
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Application of 1070-64-0,Some common heterocyclic compound, 1070-64-0, name is Ethyl 6,8-dichlorooctanoate, molecular formula is C10H18Cl2O2, 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.

600 kg (2.48 kmol) racemic 6,8-dichloroethyl caprylate and 78 kg (2.43 kmol, 0.98 equiv.) sulphur in 576 kg ethanol were placed in a 6 m3 reactor with stirrer, metering pump, pressure and internal temperature measurement and also jacket heating. At an internal temperature of 110 C. and a pressure of 0.35 MPa, 2062 kg of an aqueous sodium sulphide solution (12.3 wt. %) comprising 253.6 kg Na2S (3.24 kmol, 1.31 equiv.) was metered in uniformly with stirring over a period of 85 min. The reaction mixture was stirred for another 120 min at 110 C. Then 508 g of a solution of sodium borohydride (12 wt. %) in sodium hydroxide solution (40 wt. %) comprising 61.0 kg NaBH4 (1.61 kmol, 0.65 equiv.) was metered in uniformly within 90 min. at 70 C. The ethanol contained was distilled off from the reaction mixture to the greatest possible extent, and thereupon a further 253 kg of a solution of sodium borohydride (12 wt. %) in sodium hydroxide solution (40 wt. %) comprising 30.4 kg NaBH4 (0.80 kmol, 0.32 equiv.) added over a period of 60 min. at 70 C. Once addition had taken place, the mixture was heated to boiling and stirred further for 30 min. at this temperature. After cooling, 540 kg MTBE was added and the batch was acidified to a pH value of 2.6 to 3.0 by adding 1454 kg (12.3 kmol) hydrochloric acid (31 wt. %). The organic phase was separated off and the organic solvent was distilled off completely without a vacuum. 506 kg of a yellow liquid was obtained, with a content of 94.0 wt. % dihydrolipoic acid and a polymer content of 5.6 wt. % (corresponds to a yield of 91.8% of theory).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 6,8-dichlorooctanoate, its application will become more common.

Reference:
Patent; ALZCHEM TROSTBERG GMBH; SCHNAPPERELLE, Ingo; WINKLER, Stephan; SANS, Juergen; THALHAMMER, Franz; (7 pag.)US2019/276396; (2019); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 1070-64-0 as follows. Formula: C10H18Cl2O2

To a solution of ethyl 6,8-dichlorooctanoate (6.01 g, 25 mmol) in 95% ethanol (10mL)was added sodium hydroxide (2 g, 50 mmol) and water (38 mL). The mixture was heated to 50 C for 1.5 h and the aqueous disodium diselenide (prepared from 3.95 g selenium powder19) was then added dropwise at 65 C. After stirring for 2 h, the mixture was cooled to 40 C and activated carbon (8 g) was then added. After stirring for 0.5 h, the mixture was filtered, and the ethanol was distilled off under reduced pressure (caution: the temperatureof the filtrate must not exceed 50C). Water (400 mL) was added to the residue and the mixture was cooled to 0 C. A solution of 10% hydrochloric acid was then added dropwise till pH = 1, resulting in the formation of a solid product. The solid was filtered and washed thoroughly with water.

According to the analysis of related databases, 1070-64-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Xu, Feng; Yang, Zhen-Zhen; Zhang, Shi-Jie; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 188; 10; (2013); p. 1312 – 1319;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics