ChemicalBook CAS DataBase List 2,6-Dimethoxyphenylboronic acid

2,6-Dimethoxyphenylboronic acid synthesis

9synthesis methods

Product Name:2,6-Dimethoxyphenylboronic acid
CAS Number:23112-96-1
Molecular formula:C8H11BO4
Molecular Weight:181.98

121-43-7
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151-10-0
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23112-96-1
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$6.00/1g

Yield:23112-96-1 90%

Reaction Conditions:

Stage #1: 1,3-Dimethoxybenzenewith n-butyllithium in tetrahydrofuran;hexane at -40 - 30; for 1 h;Inert atmosphere;
Stage #2: Trimethyl borate in tetrahydrofuran;hexane at -40 - -30; for 1 h;
Stage #3: with hydrogenchloride in tetrahydrofuran;hexane;water at 20 - 30; for 1 h;

Steps:

3 Preparation of Compond II

41.5g (0.3mol) 1,3-dimethoxybenzene, 170gTHF are placed into a dry 1L three-necked flask. Under nitrogen protection, stirwhile cooling the system temperature to -30 ~ -40 deg.C. Add dropwise 240ml (0.6mol) n-butyllithium n-hexane solution. Dropping complete. Heat to 10 ~ 30 deg.C and maintain temperature for 1h. After maintaining the temperature, cool the system temperature to -30 ~ -40 deg.C. Add dropwise 62.4g (0.6mol)of trimethyl borate. Dropping complete. Maintain temperature for 1h. Maintain temperature was complete. Add 148g concentrated hydrochloric acid and 150g water. Reaction solution was stirred at 20 ~ 30 deg,C and maintain temperature 1h. Maintain temperature was completed, the reaction solution under reduced pressure until solvent-free solvent removal, the product was added to 200g of water, stirred for 20min, suction filtration using a Buchner funnel to give 45g of white solid, a yield of 90.0%, measured by gas chromatographic purity of 99.0% .

References:

CN105348240,2016,A Location in patent:Paragraph 0059; 0060

151-10-0
447 suppliers
$5.00/10g

23112-96-1
276 suppliers
$6.00/1g

References