ChemicalBook CAS DataBase List 2-Hydroxyphenylboronic acid

2-Hydroxyphenylboronic acid synthesis

15synthesis methods

Product Name:2-Hydroxyphenylboronic acid
CAS Number:89466-08-0
Molecular formula:C6H7BO3
Molecular Weight:137.93

5720-06-9 Synthesis

5720-06-9
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89466-08-0
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Yield:89466-08-0 92%

Reaction Conditions:

Stage #1:2-Methoxyphenylboronic acid with aluminum (III) chloride;acetyl chloride in toluene at 10 - 100; for 3.75 h;Large scale;
Stage #2: with hydrogenchloride in water; pH=4Large scale;

Steps:

3; 2
Use a vacuum pump to vacuum the reactor to -0.1Mpa, lower the temperature of the reactor to 10, add 1.52kg (10mol) o-methoxyphenylboronic acid, 1.57kg (20mol) acetyl chloride, and 12L toluene into the reactor and mix Stir until it is uniform, then add 2mol aluminum chloride, increase the temperature by 10 every 15 minutes during the reaction, until the temperature reaches 100, and then react at a constant temperature for 1.5h (the methyl chloride gas generated during the reaction is removed to the recovery system by vacuum ) To obtain the intermediate compound, add sodium carbonate solution to adjust the pH of the system to 10 to obtain an aqueous layer, continue to use hydrochloric acid to adjust the aqueous layer to pH 4, extract with ethyl acetate, collect the organic layer, concentrate, and re-weight with n-hexane Crystallized to obtain 1.27 kg of o-hydroxyphenylboronic acid, with a yield of 92% and a purity of 99.3%.

References:

Business Hezhiji New Materials Technology Center;Lu Zhengxiang CN112047970, 2020, A Location in patent:Paragraph 0042-0043; 0048-0049

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213211-69-9 Synthesis