Homoallyl halide composition and method for storing homoallyl halide
A composition and halide technology, applied in chemical instruments and methods, disproportionation separation/purification of halogenated hydrocarbons, organic chemistry, etc., can solve problems such as polymerization and danger
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[0036] Hereinafter, the present invention will be specifically described based on examples, but the present invention is not limited to these examples.
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[0038] Add 43.06g (0.50mol) of 3-methyl-3-buten-1-alcohol, 55.65g (0.55mol) of triethylamine, ether 200 g, and the temperature of the internal mixture was cooled to 5° C. while stirring. Then, 65.43 g (0.55 mol) of thionyl chloride was added dropwise over 2.5 hours while keeping the internal temperature at 10° C. or lower. After completion of the dropwise addition, it was heated to an internal temperature of 50 to 55° C., and heated and stirred for 13 hours. After cooling, 125 g of water was added, stirred, and left to stand, then the water phase was separated, and the organic phase was washed with 130 g of a 5% aqueous sodium bicarbonate solution and 125 g of water. 235.2 g of the separated organic phase were obtained, and the organic phase was analyzed by gas chromatography, and as a result, 46.5 g (0.44 mol; yield 88%) of 3-methyl-3-butenyl chloride were contained. The reaction liquid was distilled under reduced pressure to obtain 23.3 g of 3-methyl-3-butenyl chloride (he...
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