Synthesizing method for 3-methoxyacrylate

A technology for the synthesis of methyl methoxyacrylate, applied in the field of chemistry, can solve the problems of increased separation cost and process, high comprehensive cost of industrialization, and many steps, and achieve good product purity, reduced production cost, and fewer reaction steps Effect

Inactive Publication Date: 2016-03-23
吴清来
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material 3-methoxy-3-ethoxy propionate methyl ester used in this method is synthesized by trichloroacetyl chloride and vinyl ethyl ether, but there are many steps, wherein 3-methoxy-3-ethoxy When methyl propionate and methanol undergo alcohol exchange reaction to synthesi

Method used

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  • Synthesizing method for 3-methoxyacrylate
  • Synthesizing method for 3-methoxyacrylate

Examples

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example 1

[0028] (1) In a 500ml three-neck flask, add 182g of trichloroacetyl chloride and 300mL of dichloromethane, and cool down to -5°C to 0°C in an ice-salt bath. Slowly feed 120g of vinyl methyl ether, after ventilation is complete, stir and react at room temperature for 12 hours, take a sample and control, trichloroacetyl chloride is basically reacted completely, dichloroethane and excess vinyl methyl ether are distilled out under reduced pressure by the water pump, and then, the oil pump Distilled under reduced pressure to obtain 190g of BJ01, based on trichloroacetyl chloride, the yield was 85%.

[0029] (2) Add 190g of BJ01 and 250g of anhydrous methanol to a 1000ml three-neck flask, cool down to 0°C-10°C in an ice-salt bath, add 20g of anhydrous potassium carbonate, stir, heat to 20°C-30°C, and keep warm for 12 Hour. After the reaction is complete, cool down to room temperature, filter with suction to remove solid salts, distill the filtrate under reduced pressure with a wate...

example 2

[0032] (1) In a 500ml three-neck flask, add 182g of trichloroacetyl chloride and 300mL of cyclohexane, and cool down to -5°C to 0°C in an ice-salt bath. Slowly feed 120g of vinyl methyl ether, after ventilation is complete, stir and react at room temperature for 12 hours, take a sample to control, trichloroacetyl chloride is basically reacted completely, and the water pump depressurizes to distill out cyclohexane and excess vinyl methyl ether, then, the oil pump reduces 181gBJ01 was obtained by pressure distillation, and the yield was 81% based on trichloroacetyl chloride.

[0033] (2) In a 1000ml three-necked flask, add 181g BJ01 and 250g anhydrous methanol, cool down to 0°C-10°C in an ice-salt bath, add 20g anhydrous sodium carbonate, stir, heat to 20°C-30°C, and keep warm for 12 Hour. After the reaction is complete, cool down to room temperature, filter with suction to remove solid salts, distill the filtrate under reduced pressure with a water pump to remove methanol, and...

example 3

[0036] (1) In a 500ml three-neck flask, add 182g of trichloroacetyl chloride and 300mL of dichloromethane, and cool down to -5°C to 0°C in an ice-salt bath. Slowly feed 120g of vinyl methyl ether, after ventilation is complete, stir and react at room temperature for 12 hours, take a sample and control, trichloroacetyl chloride is basically reacted completely, dichloroethane and excess vinyl methyl ether are distilled out under reduced pressure by the water pump, and then, the oil pump Distilled under reduced pressure to obtain 188g of BJ01, based on trichloroacetyl chloride, the yield was 84.1%.

[0037] (2) Add 188g of BJ01 and 250g of anhydrous methanol to a 1000ml three-neck flask, cool down to 0°C-10°C in an ice-salt bath, add 20g of anhydrous potassium carbonate, stir, heat to 20°C-30°C, and keep warm for 12 Hour. After the reaction is complete, cool down to room temperature, filter with suction to remove solid salts, distill the filtrate under reduced pressure with a wa...

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Abstract

The present invention relates to a synthesizing method for 3-methoxy-3-ethoxy methyl propionate, and belongs to the field of chemistry. The synthesizing step comprises the following steps: introducing methyl vinyl ether into trichloroacetyl chloride, and insulating until a reaction is completed; combining BJ01 with anhydrous methanol, adding an acid-binding agent I, and insulating until a reaction is completed; and mixing BJ02 with an organic solvent 2, adding a catalyst, and insulating until a reaction is completed to obtain the 3-methoxyacrylate. The synthesizing method for the 3-methoxyacrylate has the advantages of few reaction steps, easiness in operation, less waste gas, waste water and waste residues, high yield, high purity of products, and inexpensive and easily available raw materials. All the steps have no harsh conditions and are simple in operation and environmentally-friendly, and the solvent are easily recycled and reused, so that the synthesizing method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemistry, in particular to a method for synthesizing methyl 3-methoxyacrylate. Background technique [0002] Methyl 3-methoxyacrylate is an important chemical intermediate, widely used in the fields of medicine, pesticides and polymer materials, and can be used to synthesize the herbicide fenpyrazone, the insecticide flonicamid and the pharmaceutical Ceftibuten etc., its structure is the compound shown in formula one: [0003] [0004] (Formula 1) [0005] According to domestic and foreign literature reports, at present 3-methoxymethyl acrylate mainly contains the following several synthetic methods. [0006] One: Using methyl acrylate and methanol as raw materials, under the action of catalysts such as palladium chloride, synthesize 3-methoxymethyl acrylate and 3,3-dimethoxymethyl propionate, 3,3-dimethyl Methyl oxypropionate is further cleaved to give methyl 3-methoxyacrylate. This method has a short rout...

Claims

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Application Information

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IPC IPC(8): C07C67/327C07C69/734
CPCC07C67/327C07C45/69C07C67/42C07C69/734C07C49/227C07C69/67
Inventor 吴清来鲁东飞
Owner 吴清来
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