A kind of preparation method of piperonal

A technology of piperonal and piperonyl ring, which is applied in the field of synthesis of piperonal, can solve the problems of complex operation, difficulty in purchasing, and high price, and achieve the effects of low discharge of three wastes, simplified procedures, and easy disposal

Active Publication Date: 2021-06-15
SUZHOU HOMESUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2-Nitropropane is difficult to purchase and expensive in the market
If the oxidant nitric acid is used, its consumption is relatively large, and a large amount of nitrogen oxides generated after the reaction will pollute the air; the operation is complicated, and the concentration of nitric acid or the drop rate of concentrated nitric acid must be strictly controlled.

Method used

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  • A kind of preparation method of piperonal
  • A kind of preparation method of piperonal
  • A kind of preparation method of piperonal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Add 680g of polyphosphoric acid into a 2000ml three-necked flask, add 120ml of ethanol under stirring, heat up to 55°C, slowly add 50g (0.41mol) of piperonylcycline dropwise, and finish dripping in 0.5 hours, add 60g (0.43mol) of urotropine, and add After completion, start to heat up to 90-100°C, keep it warm for 3 hours, take a sample for liquid phase analysis, cool down to 60-70°C, add 700ml of water, stir for 3 hours, add ethyl acetate twice for extraction, 650ml each time, combine the organic phases, Add 400ml of saturated brine to wash, separate the organic phase, add 40g of anhydrous sodium sulfate to dry for 1 hour, filter, the filtrate is concentrated in ethyl acetate at 40°C, and the remaining liquid is distilled under reduced pressure by an oil pump to obtain 43g of piperonal with a purity of 99%.

[0053] 1H-NMR (300MHZ): (δ6.08(s, 2H); δ6.95(d, 1H); δ7.34(s, 1H); δ7.43(d, 1H); δ9.82(s, 1H).

Embodiment 2

[0055] Add 350g of polyphosphoric acid into a 1000ml three-necked bottle, add 100ml of ethanol while stirring, heat up to 55°C, slowly add 50g of peppercycline dropwise, and finish dropping in 0.5 hours, add 60g of urotropine, after the addition is complete, start to heat up to 70°C, Keep warm for 5 hours, sample liquid phase analysis, lower the temperature to 60-70°C, add 300ml of water, stir for 3 hours, add ethyl acetate for two extractions, 400ml each time, combine the organic phase, add 300ml of saturated saline to wash, and separate the organic phase. Phase, add anhydrous sodium sulfate 30g and dry for 1 hour, filter, the filtrate is concentrated ethyl acetate at 40 ℃, and the remaining liquid is distilled under reduced pressure by an oil pump to obtain 40g of piperonal with a purity of 99%.

Embodiment 3

[0057] Add 350g of polyphosphoric acid into a 1000ml three-necked bottle, add 100ml of ethanol while stirring, heat up to 55°C, slowly add 50g of peppercycline dropwise, and finish dropping in 0.5 hours, add 60g of urotropine, after the addition is complete, start to heat up to 70°C, Insulated for 5 hours, sampled for liquid phase analysis, concentrated ethanol under reduced pressure, and distilled under reduced pressure by an oil pump to obtain 32 g of piperonal with a purity of 97%.

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Abstract

The invention provides a preparation method of piperonal, comprising: reacting piperonyl cycline, a catalyst and urotropine in an alcohol solvent at 50-120° C. for 1-10 hours to obtain piperonal. The overall process only needs one-step reaction, the process is simplified, the yield is high, the discharge of three wastes is relatively low, the waste water is easy to treat, and it is easy to realize industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for synthesizing piperonal. Background technique [0002] Piperonal, chemical name is 3,4-methylenedioxybenzaldehyde, molecular formula is C 8 h 6 o 3 , white to light yellow crystals. Soluble in general organic solvents, insoluble in water and glycerin. The melting point is 35-37°C, and the boiling point is 261-263°C. Piperonal not only has a sweet heliotrope aroma, but also has a light and slightly sweet cherry and sunflower aroma, and also has a faint spicy aroma, which lasts for a long time. The deployment of flavors. [0003] The method for preparing piperonal has following several at present: [0004] (1) take piperine as the synthesis of raw material: [0005] The method uses piperine and alkali solution to heat to obtain piperic acid, and then oxidizes with potassium permanganate to obtain piperonal. This process has rare raw materials and hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/54
CPCC07D317/54
Inventor 翟金星黄勇陆红彬樊超
Owner SUZHOU HOMESUN PHARMA
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