ChemicalBook CAS DataBase List 3,4-Dimethoxyphenol

3,4-Dimethoxyphenol synthesis

9synthesis methods

Product Name:3,4-Dimethoxyphenol
CAS Number:2033-89-8
Molecular formula:C8H10O3
Molecular Weight:154.16

120-14-9 Synthesis

120-14-9
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$5.00/25g

2033-89-8
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$15.00/1g

Yield:2033-89-8 96%

Reaction Conditions:

Stage #1:3,4-dimethoxy-benzaldehyde with 3-chloro-benzenecarboperoxoic acid in dichloromethane at 20; for 15 h;
Stage #2: with potassium carbonate in methanol at 20; for 0.5 h;

Steps:

3,4-dimethoxyphenol (Compound 3)
Chloroperbenzoic acid (2.23 g with 77%, ca. 9.93 mmol) was added to a solution of 3,4-dimethoxybenzaldehyde (Compound 2) (1.50 g, 9.03 mmol) dissolved in CH2Cl2 (25 mL) Was stirred at room temperature for 15 hours. The reaction mixture was quenched by the addition of dimethyl sulfide (1 mL) and washed with a saturated aqueous solution of Na2SO3 (3 x 20 mL) and brine (20 mL). The organic solvent phase was dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was dissolved in methanol (23 mL) and then treated with K2CO3 (2.49 g, 18.05 mmol) and the mixture was stirred at room temperature for 30 min. After removal of the methanol, the residue was dissolved in EtOAc (30 mL), washed with H2O (2 x 15 mL), brine (15 mL) and dried over anhydrous Na2SO4. The organic solvent phase was filtered and concentrated, and the residue was purified by column chromatography (EtOAc / hexane = 1/1) to give a white solid compound 3 (1.34 g, 96%).

References:

Hallym University Industry-Academic Cooperation Foundation;Jeon, Chung Gab;Kongara, Damodar KR101740915, 2017, B1 Location in patent:Paragraph 0053-0054

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