Method for preparing chlorophenylboronic acid
A technology of p-chlorophenylboronic acid and chlorobromobenzene, which is applied in the field of preparation of p-chlorophenylboronic acid, can solve the problems of complicated operation and low yield, and achieve the effects of shortening the reaction cycle, high yield and less by-products
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Embodiment １
[0023] The present embodiment provides a kind of preparation method of p-chlorophenylboronic acid, it comprises the following steps:
[0024] 1) Under the protection of nitrogen, add 314g toluene to the 1L reaction flask, then add 382g p-chlorobromobenzene, stir well to obtain solution A;
[0025] 2) Under the protection of nitrogen, add 160g of tetrahydrofuran to the 1L reaction flask, then add 207.8g of trimethyl borate, stir well to obtain solution B;
[0026] 3) Under the protection of nitrogen, add 314g of tetrahydrofuran, 48.6g of magnesium chips and 0.5g of iodine particles into the 2L reaction flask, add the solution B under stirring, heat up to 40-50°C in a water bath, and then use 3mL / min The solution A was added dropwise at a high rate, and after the dropwise addition was completed, the reaction was incubated for 2.5 hours;
[0027] 4) Transfer the reaction mixture to a 3L reaction bottle, slowly add 18% dilute hydrochloric acid dropwise to pH 2-3 under stirring, k...
Embodiment 2
[0030] The present embodiment provides a kind of preparation method of p-chlorophenylboronic acid, it comprises the following steps:
[0031] 1) Under the protection of nitrogen, add 568g of toluene to the 1L reaction flask, then add 382g of p-chlorobromobenzene, stir well to obtain solution A;
[0032] 2) Under the protection of nitrogen, add 279g tetrahydrofuran to the 1L reaction flask, then add 207.8g tripropyl borate, stir well to obtain solution B;
[0033] 3) Under the protection of nitrogen, add 316g of tetrahydrofuran, 48.6g of magnesium chips and 0.5g of iodine particles into the 2L reaction flask, add the solution B under stirring, heat up to 40-50°C in a water bath, and then add the solution B at 3mL / min The solution A was added dropwise at a high rate, and after the dropwise addition was completed, the reaction was incubated for 2.5 hours;
[0034] 4) Transfer the reaction mixture to a 3L reaction bottle, slowly add 18% dilute hydrochloric acid dropwise to pH 2-3...
Embodiment 3
[0037] The present embodiment provides a kind of preparation method of p-chlorophenylboronic acid, it comprises the following steps:
[0038] 1) Under nitrogen protection, add 402g of methyl tert-butyl ether to a 1L reaction flask, then add 382g of p-chlorobromobenzene, stir well to obtain solution A;
[0039] 2) Under the protection of nitrogen, add 226g of methyl tetrahydrofuran to the 1L reaction flask, then add 205g of triisobutyl borate, stir evenly, and obtain solution B;
[0040] 3) Under the protection of nitrogen, add 313g of tetrahydrofuran, 48.6g of magnesium chips and 0.5g of iodine pellets into a 2L reaction flask, add the solution B under stirring, heat up to 40-50°C in a water bath, and then use 3mL / min The solution A was added dropwise at a high rate, and after the dropwise addition was completed, the reaction was incubated for 2.5 hours;
[0041] 4) Transfer the reaction mixture to a 3L reaction bottle, slowly add 18% dilute hydrochloric acid dropwise to pH 2...
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