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ChemicalBook CAS DataBase List 1-Chloro-6,6-dimethyl-2-heptene-4-yne
126764-17-8

1-Chloro-6,6-dimethyl-2-heptene-4-yne synthesis

1synthesis methods
-

Yield:-

Reaction Conditions:

with hydrogenchloride;trichlorophosphate in water;acetonitrile at 10 - 28; for 6.33333 h;

Steps:

2
30 kg of pure 6,6-dimethyl-1-heptene-4-yne-3-ol obtained in Example 1 was taken into a reactor containing 103 liters of acetonitrile under stirring. The mass was cooled to 10 °C and a homogeneous mixture of 7.1 liters of phosphorous oxychloride in 52 liters of aqueous hydrochloric acid was added to the mass slowly at 12 0C. The mass was maintained at this same temperature for 60 minutes and then the temperature was raised to 25 °C. Temperature was maintained at 28 0C for 5 hours and then 130 liters of water was charged. The mass was stirred for 20 minutes and was extracted three times with petroleum ether (3*90 liters). The combined organic layers were washed with water (4*100 liters) and the solvent was distilled completely below 80 °C to get 42.8 kg of the title compound as a residue.The residue thus obtained was charged into a clean and dry reactor and was purified by fractional distillation. The main fraction was collected at 57-98 °C under reduced pressure of 30-60 torr to get 22.2 kg of the purified 1-chloro-6,6- dimethyl-2-heptene-4-yne.

References:

DR. REDDY'S LABORATORIES LTD.;DR. REDDY'S LABORATORIES, INC. WO2007/44273, 2007, A1 Location in patent:Page/Page column 16

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