CN105646167A - Synthetic process for p-methoxybenzaldehyde - Google Patents
Synthetic process for p-methoxybenzaldehyde Download PDFInfo
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- CN105646167A CN105646167A CN201410626270.3A CN201410626270A CN105646167A CN 105646167 A CN105646167 A CN 105646167A CN 201410626270 A CN201410626270 A CN 201410626270A CN 105646167 A CN105646167 A CN 105646167A
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- aubepine
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Abstract
The invention discloses a synthetic process for p-methoxybenzaldehyde. The synthetic process comprises methylation reaction with p-hydroxybenzaldehyde as a raw material, methyl chloride gas as a methylation raw material and water as a solvent according to a certain feeding proportion. According to the invention, methyl chloride gas is used as the methylation raw material, so reaction is single; selectivity is up to 95%; yield of a target product reaches more than 90%; meanwhile, treatment of three wastes is simple, so the process belongs to clean and green chemical synthetic process.
Description
Technical field
The invention belongs to technical field of chemical synthesis, it is specifically related to the synthesis technique of a kind of aubepine.
Background technology
Aubepine, is colourless to weak yellow liquid under normal temperature, has the smell of similar hawthorn. The main body spices of allotment hawthorn floral type. Also can be used for Syringa oblata Lindl., orchid, sunflower, Acacia, bashfully flower, locust tree, yulan, the fragrant floral type such as rowland, sweet Tofu pudding and newly cut in the non-flower pattern essence such as grass, fragrant common vetch, aldehyde perfume. Also can be used in the heavy wood flavor essences such as santal. Also in soap compound. In food with its sweet taste and be in harmonious proportion fragrance. In the technological process method preparing aubepine at present, technical process is not easy to implement, and the aubepine finished product purity of generation is low, reactant per pass conversion is low, production process is complicated, and production efficiency is low and cost height, is not suitable for scale operation.
Summary of the invention
In order to overcome the above-mentioned technical problem that prior art exists, it is an object of the present invention to provide the synthesis technique of a kind of aubepine, the present invention not only production process simple, increase work efficiency, and the aubepine product purity generated is big, it is applicable to suitability for industrialized production.
The synthesis technique of aubepine provided by the invention, comprises the following steps:
(1) taking p-Hydroxybenzaldehyde as raw material, taking monochloro methane gas as methyl raw material, water is solvent, carries out methylation reaction by certain charge ratio;
(2) utilizing alkaline matter control reaction system PH at 7.5-13.5, methylation reaction pressure is 0.05-0.5MPa, and temperature of reaction is 35-110 DEG C, and the time is that direct gas-liquid phase reaction in 2-8 hour obtains aubepine crude product (organic layer);
(3) being separated organic layer and water layer, water layer aromatic hydrocarbon (such as toluene) extracts two times, merges organic layer, and washing organic layer is to PH6.5-7.5;
(4) air distillation recycling design, then rectification under vacuum collects evaporating point of 90-93 DEG C/500-600Pa, is product aubepine.
The synthesis technique of aubepine provided by the invention, its useful effect is, overcoming prior art, to prepare operation in the technological process of aubepine more, the problem that workload is big, it is to increase working efficiency; Improve the per pass conversion of reactant and the product rate of resultant.
Embodiment
Below in conjunction with an embodiment, the synthesis technique of aubepine provided by the invention is described in detail.
Embodiment
The synthesis technique of the aubepine of the present embodiment, comprises the following steps:
(1) taking p-Hydroxybenzaldehyde as raw material, taking monochloro methane gas as methyl raw material, water is solvent, carries out methylation reaction by certain charge ratio;
(2) utilizing alkaline matter control reaction system PH 13.5, methylation reaction pressure is 0.5MPa, and temperature of reaction is 110 DEG C, and the time is that direct gas-liquid phase reaction in 8 hours obtains aubepine crude product (organic layer);
(3) being separated organic layer and water layer, water layer aromatic hydrocarbon (such as toluene) extracts two times, merges organic layer, and washing organic layer is to PH6.5;
(4) air distillation recycling design, then rectification under vacuum collects evaporating point of 93 DEG C/600Pa, is product aubepine.
The synthesis technique of aubepine, it is not necessary to process further, operation is simple, and data accurately are easy to collect, and technical process is easy to implement, it is achieved that the suitability for industrialized production of product.
Claims (1)
1. the synthesis technique of an aubepine, it is characterised in that: described method comprises the following steps:
(1) taking p-Hydroxybenzaldehyde as raw material, taking monochloro methane gas as methyl raw material, water is solvent, carries out methylation reaction by certain charge ratio;
(2) utilizing alkaline matter control reaction system PH at 7.5-13.5, methylation reaction pressure is 0.05-0.5MPa, and temperature of reaction is 35-110 DEG C, and the time is that direct gas-liquid phase reaction in 2-8 hour obtains aubepine crude product (organic layer);
(3) being separated organic layer and water layer, water layer aromatic hydrocarbon (such as toluene) extracts two times, merges organic layer, and washing organic layer is to PH6.5-7.5;
(4) air distillation recycling design, then rectification under vacuum collects evaporating point of 90-93 DEG C/500-600Pa, is product aubepine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410626270.3A CN105646167A (en) | 2014-11-10 | 2014-11-10 | Synthetic process for p-methoxybenzaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410626270.3A CN105646167A (en) | 2014-11-10 | 2014-11-10 | Synthetic process for p-methoxybenzaldehyde |
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| Publication Number | Publication Date |
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| CN105646167A true CN105646167A (en) | 2016-06-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410626270.3A Pending CN105646167A (en) | 2014-11-10 | 2014-11-10 | Synthetic process for p-methoxybenzaldehyde |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187725A (en) * | 2016-07-05 | 2016-12-07 | 上海应用技术学院 | Hydroxy benzaldehyde and the etherification method of derivant thereof |
| CN110590519A (en) * | 2019-09-25 | 2019-12-20 | 万香科技股份有限公司 | Preparation method of anisaldehyde |
-
2014
- 2014-11-10 CN CN201410626270.3A patent/CN105646167A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187725A (en) * | 2016-07-05 | 2016-12-07 | 上海应用技术学院 | Hydroxy benzaldehyde and the etherification method of derivant thereof |
| CN106187725B (en) * | 2016-07-05 | 2019-02-22 | 上海应用技术学院 | The etherification method of parahydroxyben-zaldehyde and its derivative |
| CN110590519A (en) * | 2019-09-25 | 2019-12-20 | 万香科技股份有限公司 | Preparation method of anisaldehyde |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160608 |
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| WD01 | Invention patent application deemed withdrawn after publication |