ChemicalBook CAS DataBase List 2,3,4-Trimethoxybenzaldehyde

2,3,4-Trimethoxybenzaldehyde synthesis

9synthesis methods

Product Name:2,3,4-Trimethoxybenzaldehyde
CAS Number:2103-57-3
Molecular formula:C10H12O4
Molecular Weight:196.2

2,3,4-Trimethoxybenzaldehyde is an important pharmaceutical intermediate in the synthesis of new drug Ca2+ channel blockers. It can be synthesized by methylation reaction through O-alkylation method, using 2,3,4-trihydroxybenzaldehyde as raw material, dimethyl sulfate as alkylating agent, with phase transfer catalyst quaternary ammonium salt and sodium hydroxide.

50-00-0 Synthesis

50-00-0
900 suppliers
$10.00/25g

634-36-6
343 suppliers
$7.00/5g

2103-57-3
523 suppliers
$9.00/10g

Yield:2103-57-3 82.9%

Reaction Conditions:

with potassium carbonate;magnesium chloride for 5 h;Reflux;Concentration;

Steps:

1 Example 1
The organic layer containing the intermediate (III) obtained above was placed in a 500 ml reaction flask, anhydrous magnesium chloride (13.5 g, 0.23 mol) was added, 35.4 g of paraformaldehyde was added in batches, and the dropwise addition was started. (38.6g, 0.28mol) potassium carbonate, after completion of the addition, heated to reflux, the reaction for 5 hours, the reaction solution was cooled to room temperature after the reaction was completed, then the reaction solution was slowly added dropwise to the amount of water, stirring was maintained for 30 minutes, static The layers are separated, the organic layer is collected, the organic layer is depressurized and the solvent is removed, and the fraction is collected by distillation under reduced pressure. The fraction is cooled and becomes white crystal (I) 24.4 g. The total yield is 82.9%. Purity (HPLC area normalization method) 99.6%.

References:

Jiangsu Tong He Pharmaceutical Co., Ltd.;Lu Huigang;Gong Lifeng;Gu Ye;Yuan Yuehua;Zou Zhenrong CN107382690, 2017, A Location in patent:Paragraph 0021; 0022; 0024; 0026; 0028

2144-08-3 Synthesis