3-bromomethyl-2-halo-4-alkylsulfonylbenzoate preparation method
A technology of alkylsulfonyl benzoate and bromomethyl is applied in the field of preparation of 3-bromomethyl-2-halo-4-alkylsulfonyl benzoate, and can solve the problem of high cost, Achieving the effect of low price and high yield
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[0012] The invention provides a preparation method of 3-bromomethyl-2-halo-4-alkylsulfonyl benzoate shown in formula (1), characterized in that the method comprises: In the presence of an agent, the compound shown in formula (2) is contacted with the compound shown in formula (3) and the compound shown in formula (4);
[0013]
[0014] Among them, R 1 for C 1 -C 7 straight-chain or branched-chain hydrocarbon group; R 2 and R 5 Each independently is Li, Na or K; R 3 is F, Cl or Br; R 4 for C 1 -C 5 of alkyl.
[0015] In formula (2), R 1 for C 1 -C 7 The linear or branched hydrocarbon group, for example, can be methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, n-pentyl or n-hexyl. Preferably, R 1 for C 1 -C 3 The linear or branched chain hydrocarbon group, for example, can be methyl, ethyl or isopropyl.
[0016] In formula (2), R 3 is F, Cl or Br; preferably, R 3 is Cl or Br; more preferably, R 3 for Cl.
[0017] In formula (2), R 4 for C...
Embodiment 1
[0051] Add 30g (0.112mol) methyl 2-chloro-3-methyl-4-methylsulfonylbenzoate and 120g chlorobenzene into a 500mL four-necked reaction flask; dissolve 6.8g (0.045mol) sodium bromate in In 60g of water, an aqueous solution of sodium bromate was obtained, 11.6g (0.112mol) of sodium bromide was dissolved in 60g of water, an aqueous solution of sodium bromide was obtained, and the aqueous solution of sodium bromate and aqueous solution of sodium bromate were added to the above-mentioned 500mL four-necked reaction flask Inside; under stirring, the temperature was raised to 80°C, and 0.93g (0.006mol) of azobisisobutyronitrile was added into a 500mL four-necked reaction flask; ), the dropwise addition was completed in 3 hours; after the dropwise completion, the stirring reaction was kept at 80°C for 1 hour, then the layering was allowed to stand while hot, and the water phase was separated; a small amount of sodium bisulfite aqueous solution was added to the organic phase for washing on...
Embodiment 2
[0053] Add 31.57g (0.112mol) ethyl 2-chloro-3-methyl-4-methylsulfonylbenzoate and 94.71g chlorobenzene into a 500mL four-necked reaction flask; dissolve 5.61g (0.034mol) potassium bromate in In 20g of water, potassium bromate aqueous solution was obtained; 7.5g (0.0728mol) sodium bromide was added to 30g of water to obtain sodium bromide aqueous solution, and potassium bromate aqueous solution and sodium bromide aqueous solution were added in a 500mL four-necked reaction flask; under stirring, the temperature was raised to 90 ℃, add 3.16g (0.019mol) of azobisisobutyronitrile into a 500mL four-necked reaction flask; at 90℃, add 41.16g (0.084mol) of 20% sulfuric acid aqueous solution dropwise while stirring, and the dropwise addition is completed in 4 hours ;After dropping, keep stirring and reacting at 90°C for 0.5 hours, then stand still while hot and separate the water phase; The solvent was recovered, and the obtained solid was recrystallized by adding ethanol to obtain 37.3...
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