Method for synthesizing 1-(3-ethyoxyl-4-methoxy)phenyl-2-methyl-sulfonyl ethylamine
A technology of methanesulfonylethylamine and methyl methoxybenzoate, which is applied in the field of organic synthesis technology, can solve the problems of high price of benzoate, multiple temperature change steps, difficult control, etc., and achieve stable and low-cost raw materials , low cost, route safety and environmental protection
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Embodiment 1
[0037] (1) Preparation of 3-hydroxyl-4-methoxybenzoic acid methyl ester
[0038] Add 15g of 3-hydroxy-4-methoxybenzoic acid, 165ml of methanol, and 540uL of concentrated sulfuric acid to a dry 100mL three-necked flask in sequence, raise the temperature to 55°C, and react overnight under magnetic stirring. Thin-layer chromatography was used to determine the reaction progress, and the developing solvent was ethyl acetate:dichloromethane=1:1. After the completion of the reaction, collect the product, and transfer the product to a round bottom flask for distillation under reduced pressure to remove methanol, extract the residue with 20 mL of ethyl acetate, and add 10 mL of saturated sodium bicarbonate solution for neutralization, take the organic phase, and depressurize Ethyl acetate was distilled off to obtain 11.86 g of solid product methyl 3-hydroxy-4-methoxybenzoate, yield 67.7%.
[0039] (2) Preparation of 3-ethoxyl-4-methoxybenzoic acid methyl ester
[0040] Add 10.36g of ...
Embodiment 2
[0046] (1) Preparation of 3-hydroxyl-4-methoxybenzoic acid methyl ester
[0047] Add 10g of 3-hydroxy-4-methoxybenzoic acid, 110ml of methanol, and 360uL of concentrated sulfuric acid to a dry 100mL three-necked flask in sequence, raise the temperature to 65°C, and react overnight under magnetic stirring. Thin-layer chromatography was used to determine the reaction progress, and the developing solvent was ethyl acetate:dichloromethane=1:1. After the completion of the reaction, collect the product, and transfer the product to a round bottom flask for distillation under reduced pressure to remove methanol, extract the residue with 25 mL of ethyl acetate, and add 15 mL of saturated sodium bicarbonate solution for neutralization, take the organic phase, and depressurize Ethyl acetate was distilled off to obtain 9.06 g of solid product methyl 3-hydroxy-4-methoxybenzoate with a yield of 83.6%.
[0048] (2) Preparation of 3-ethoxyl-4-methoxybenzoic acid methyl ester
[0049] Add 10...
Embodiment 3
[0055] (1) Preparation of 3-hydroxyl-4-methoxybenzoic acid methyl ester
[0056] Add 5g of 3-hydroxy-4-methoxybenzoic acid, 55ml of methanol, and 180uL of concentrated sulfuric acid to a dry 100mL three-necked flask in sequence, raise the temperature to 70°C, and react overnight under magnetic stirring. Thin-layer chromatography was used to determine the reaction progress, and the developing solvent was ethyl acetate:dichloromethane=1:1. After the completion of the reaction, collect the product, and transfer the product to a round-bottomed flask for distillation under reduced pressure to remove methanol, extract the residue with 15 mL of ethyl acetate, and add 8 mL of saturated sodium bicarbonate solution for neutralization, take the organic phase, and depressurize Ethyl acetate was distilled off to obtain 4.67 g of a solid product, methyl 3-hydroxy-4-methoxybenzoate, with a yield of 80.1%.
[0057] (2) Preparation of 3-ethoxyl-4-methoxybenzoic acid methyl ester
[0058] Add...
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