Preparation process of vertraldethyde

A preparation process and a technology for veratroaldehyde, applied in the field of preparation technology of veratroaldehyde, can solve the problems of unstable yield, unsuitable control of bromination, and many by-products, and achieve the advantages of reducing production cost, saving time, and improving yield. Effect

Inactive Publication Date: 2012-01-18
SHANDONG HOLLY PHARM CO LTD
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  • Abstract
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Problems solved by technology

Although the price of the main raw material in this method is not expensive, the bromination should not be controlled, resulting in unstable yield and many by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: In the 2000ml of four-

[0018] Add 350g of veratrole into the flask, start stirring, then add 345g of phosphorus oxychloride, when the temperature rises to 30°C, start to add 280g of N-methylformanilide dropwise, control the temperature at 30-90°C, about 2 The addition was completed in -6 hours, and the reaction was continued at 30-90°C after the addition was completed. Add 1000ml of toluene to a 3000ml flask for later use. After qualified, transfer the material to a 3000ml flask filled with toluene, slowly add 1000ml of water under stirring, control the addition temperature at 65-85°C, continue to hydrolyze at 65-85°C for 2-6 hours after the addition, stand still, and separate layers , the water layer is added with alkali to recover raw materials; the oil layer is concentrated, toluene is evaporated, and the residue is simply rectified in a high vacuum. First, the unreacted veratrol is received, and then the finished veratraldehyde is received. White to ...

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PUM

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Abstract

The invention discloses a preparation process of vertraldethyde; veratrole is used as a main synthetic raw material and a solvent; a formylation reaction is performed by veratrole and a complex generated by N-methylformanilide and phosphorus oxychloride; a product is obtained after hydrolyzation; the using amount of the solvent during the reaction is reduced, and the yield of a single batch is increased. Meanwhile, a lot of veratrole and N-methylaniline can be recovered for recycle, which reduces the production cost to a large extent. In addition, the charging temperature is increased, and thus complexation and the formylation reaction can be performed simultaneously, which saves a lot of time; and the product after distillation has purity of up to above 99%.

Description

technical field [0001] The invention specifically relates to a preparation process of veratraldehyde. Background technique [0002] Veratraldehyde (Veratraldehyde), also known as methyl vanillin, methyl vanillin, chemical name: 3,4-dimethoxybenzaldehyde, molecular formula C 9 h 10 o 3 , is a synthetic spice with a vanilla-like aroma, and is also a pharmaceutical intermediate with many uses. It is not only an important intermediate in the synthesis of dopa drugs, such as levodopa L-DOPA, but also can be used to synthesize the anti-allergic drug Tranicob, the antihypertensive drug prazosin and tetrahydropalmatate for the treatment of arthritis. The adrenaline β-receptor blocker veratramine that is selective for the heart, the drug resantamyl used to prevent allergic asthma and allergic rhinitis, and can also be used to synthesize some important pharmaceutical intermediates such as 6.7- Dimethoxy-2-styrene quinoline, 6.7-dimethoxy-2.4 dihydroxyquinazoline, N.N'-bis(3.4-dim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/575C07C45/45
Inventor 李兰花裘月南沈林华蔺珍
Owner SHANDONG HOLLY PHARM CO LTD
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