Synthetic Route of 2009-83-8 , The common heterocyclic compound, 2009-83-8, name is 6-Chlorohexan-1-ol, molecular formula is C6H13ClO, 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.
A three-necked reactor equipped with a condenser and a thermometer was charged with hydroquinone 104.77 g (0.9515 mol), 100 g (0.7320 mol) of 6-chlorohexanol, 500 g of distilled water and 100 g of o-xylene were added. While stirring the whole volume, 35.15 g (0.8784 mol) of sodium hydroxide was further added in small portions over 20 minutes so that the temperature of the contents did not exceed 40 C. After completion of the addition of sodium hydroxide, the contents were heated and the reaction was further carried out under reflux conditions (96 C.) for 12 hours After completion of the reaction, the temperature of the reaction solution was lowered to 80 C., 200 g of distilled water was added, and then the reaction solution was cooled to 10 C. to precipitate crystals. Precipitated crystals were separated by solid-liquid separation by filtration, and the obtained crystals were washed with 500 g of distilled water and vacuum dried to obtain 123.3 g of brown crystals. Analysis of this brown crystal by high performance liquid chromatography revealed that the content ratio (molar ratio) of the compound contained in the brown crystal is (hydroquinone / intermediate K / by-product K = 1.3 / 90.1 / 8. 1). This mixture was directly used for step 2 without purification.
The synthetic route of 2009-83-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ZEON CORPORATION; SAKAMOTO, KEI; OKUYAMA, KUMI; KIRIKI, SATOSHI; (83 pag.)JP2017/206490; (2017); A;,
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