Synthesis method of 2, 4-dichlorophenoxyacetic acid compound
A technology of dichlorophenoxyacetic acid compound and dichlorophenoxyacetic acid ester, which is applied in 2 fields, can solve the problems of unfavorable industrial production, many chlorinated by-products, and incomplete conversion, so as to avoid post-processing difficulties and reaction conversion Efficiency increase, avoid hydrolysis effect
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specific Embodiment approach 1
[0014] Specific embodiment one: a kind of 2 of the present embodiment, the synthetic method of 4-dichlorophenoxyacetic acid compound, it is to carry out according to the following steps:
[0015] 1. Add 2,4-dichlorophenol into the reaction flask, then add anhydrous carbonate weak base, haloacetate and catalyst; start stirring after heating and melting, and carry out condensation reaction. HPLC monitors until there is no 2,4 -Dichlorophenol, stop reaction; Obtain intermediate 2,4-dichlorophenoxyacetate;
[0016] 2. Add water to the intermediate 2,4-dichlorophenoxyacetate, heat to reflux for hydrolysis reaction, monitor to no 2,4-dichlorophenoxyacetate by HPLC, cool, add acid solution to carry out acidification reaction, After the reaction, it was lowered to room temperature, filtered, washed, and dried to obtain a white solid of 2,4-dichlorophenoxyacetic acid.
[0017] The yield of 2,4-dichlorophenoxyacetic acid obtained in this embodiment is more than 97%, the effective conte...
specific Embodiment approach 2
[0018] Embodiment 2: This embodiment differs from Embodiment 1 in that the molar ratio of 2,4-dichlorophenol to haloacetate is 1:1.2-2.0.
[0019] Others are the same as in the first embodiment.
[0020] The molar ratio of the haloacetate compound to 2,4-dichlorophenol in this embodiment is preferably 1.3˜1.5:1.0.
specific Embodiment approach 3
[0021] Embodiment 3: This embodiment differs from Embodiment 1 in that: the catalyst is one or more of polyether, crown ether, and quaternary ammonium salt.
[0022] Others are the same as in the first embodiment.
[0023] The catalyst described in this embodiment is preferably one or more of polyethylene glycols, 15-crown-4, benzyltrimethylammonium salt and tetrabutylammonium salt; more preferably polyethylene glycol di Methyl ether, tetrabutylammonium bromide salt.
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