Allyl chloride → Allyl chloride

関与物質

反応手順

In the preferred embodiment of this invention for the production of DATBP, 1 mole of tetrabromophthalic anhydride, 0.55 mole of sodium carbonate (or 1 mole of sodium hydroxide) and a catalytic amount (0.024 mole) of triethylamine are added to a large excess (up to 10-20 moles) of allyl alcohol as a solvent as well as a reactant. If sodium hydroxide is used as the base, it is convenient to dissolve it in the allyl alcohol before the addition of the tetrabromophthalic anhydride. The mixture is stirred and heated to 90° C.-95° C. to speed the reaction to completion, yielding a solution or a thin suspension of the sodium salt of monoallyl tetrabromophthalate. After the completion of this step, 1.2 moles of allyl chloride plus a catalytic amount (0.33 mole) of allyltriethylammonium chloride (either preformed or formed in situ from triethylamine and additional allyl chloride) are added and the mixture is heated in a closed vessel for 2 hours at 100° C.-110° C., developing an equilibrium pressure of 103 kPa-172 kPa (15-25 psig). Longer heating may be required if no pressure is allowed to develop. On cooling, the DATBP crystallizes and the separated product requires only washing with cold water and drying to assay 94% to 98%. The washing may be accomplished by merely spraying with water in a centrifuge.

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