Synthesis of substituted methyl benzylketone

A synthetic method and technology of phenylacetone, applied in the direction of organic chemical methods, chemical instruments and methods, oxidation preparation of carbonyl compounds, etc., can solve the problems of high cost and low yield, and achieve wide application, high yield, and raw material Easy to get effect

Active Publication Date: 2009-02-18
YIYUAN XINQUAN CHEM +1
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  • Application Information

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Benefits of technology

This patented process allows people to easily create chemicals called phenylpropanones that are useful because they have many benefits such as being easier-to-produce or less harmful than other methods like acrylic acid.

Problems solved by technology

The technical problem addressed in this patents relating to improving the efficiency or yielding of certain chemicals used during their production process is finding ways to make them more efficiently without requiring expensive starting materials like Phenol Ampicillin Glycerate (PAAG).

Method used

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  • Synthesis of substituted methyl benzylketone
  • Synthesis of substituted methyl benzylketone

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Embodiment 1

[0018] Embodiment 1: the synthesis of phenylacetone

[0019] In a three-necked reaction flask equipped with a reflux condenser, a nitrogen inlet and outlet, and a magnetic stirrer, add 300 mL of pure tetrahydrofuran, 17.0 g of magnesium powder, 67.5 g of chlorinated benzene, and several grains of iodine. Slowly heated to 65° C. under stirring in a nitrogen flow, and reacted at a constant temperature for 1 hour, then heated to 75° C., and reacted at a constant temperature for 4 hours. Cool the reaction solution to -5°C with ice water, slowly drop 45.0g of propylene oxide into the reaction solution from the dropping funnel, after dropping, keep stirring at 0°C for 1 hour, then naturally raise the temperature to 20°C, and stir for 0.5 Hour. After the reaction solution was post-treated by the usual method, 74.4 g of the product was obtained by distillation under reduced pressure, which was identified as 1-phenyl-2-propanol by GC-MS, with a purity of 99.1% and a yield of 91%.

[...

Embodiment 2

[0021] Embodiment 2: the synthesis of p-methoxyphenylacetone

[0022] In a three-neck reaction flask equipped with a reflux condenser, nitrogen inlet and outlet, and a magnetic stirrer, add 300mL of pure tetrahydrofuran, 17.0g of magnesium powder, 85.5g of p-methoxychlorobenzene, and several grains of iodine. Slowly heated to 65° C. under stirring in a nitrogen flow, and reacted at a constant temperature for 1 hour, then heated to 75° C., and reacted at a constant temperature for 4 hours. Cool the reaction solution to -5°C with ice water, slowly drop 45.0g of propylene oxide into the reaction solution from the dropping funnel, after dropping, keep stirring at 0°C for 1 hour, then naturally raise the temperature to 20°C, and stir for 0.5 Hour. After the reaction solution was post-treated by the usual method, 87.7 g of the product was obtained by distillation under reduced pressure, which was identified as 1-(p-methoxyphenyl)-2-propanol by GC-MS, with a purity of 98.0% and a yi...

Embodiment 3

[0024] Embodiment 3: the synthesis of p-fluorophenylacetone

[0025] In a three-necked reaction flask equipped with a reflux condenser, nitrogen inlet and outlet, and a magnetic stirrer, add 300 mL of pure tetrahydrofuran, 17.0 g of magnesium powder, 103.0 g of p-fluorobromobenzene, and several grains of iodine. Slowly heated to 65° C. under stirring in a nitrogen flow, and reacted at a constant temperature for 1 hour, then heated to 75° C., and reacted at a constant temperature for 4 hours. Cool the reaction solution to -5°C with ice water, slowly drop 45.0g of propylene oxide into the reaction solution from the dropping funnel, after dropping, keep stirring at 0°C for 1 hour, then naturally raise the temperature to 20°C, and stir for 0.5 Hour. After the reaction solution was post-treated by the usual method, 75.8 g of the product was obtained by distillation under reduced pressure, which was identified as 1-(p-fluorophenyl)-2-propanol by GC-MS, with a purity of 98.0% and a ...

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Abstract

The invention provides a method for synthesizing substituted phenyl acetone. Halide aryl compound reacts with magnesium powder to produce Grignard reagent aryl magnesium halide; the aryl magnesium halide reacts with propylene oxide to produce 1-aryl-2-propanol; the 1-aryl-2-propanol reacts with oxydol under the catalyst of sodium tungstate and quaternary ammonium salt to produce 1-substituted phenyl acetone. In the method, the material is easily obtained, the process is simple and practical and the overall yield of the product reaches 83 percent.

Description

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Claims

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Application Information

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Owner YIYUAN XINQUAN CHEM
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