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Synthesis method of 4-bromophenyl allyl ether

The technology of a bromophenyl allyl ether and a synthetic method is applied in directions such as ether preparation, ester reaction preparation of ether, organic chemistry, etc., and can solve problems such as large side reactions, unsatisfactory product yield and purity, and the like, Achieve improved yield and purity and avoid separation difficulties

Inactive Publication Date: 2018-12-14
杨程飞扬
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually in the case of no phase transfer catalyst in the water phase, this side reaction is relatively large, making the yield and purity of the product less than ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1, a kind of synthetic method of intermediate p-bromophenyl allyl ether, it is characterized in that the method comprises the following steps:

[0019] Step 1, add 15g sodium bromide, 5g anhydrous potassium carbonate, 0.5g catalyst Bi in the 100ml four-neck flask with mechanical stirrer 2 OS 2 / Nb 6 o 17 -NH 3 and 30ml of acetone, stir and heat up to 45°C, and keep it for 30min after it is completely dissolved;

[0020] Step 2. Slowly add 36g of p-bromophenol and 8g of chloropropene under vigorous stirring. At this time, the temperature is controlled at 50°C, and the reaction is refluxed at 80°C for 3h after the dropwise addition;

[0021] Step 3. Cool to room temperature after the reaction, filter with suction, distill at normal pressure to obtain acetone, neutralize with dilute hydrochloric acid solution, wash with water until PH = 7, and collect fractions at about 160°C by vacuum distillation to obtain a colorless transparent liquid.

[0022] The Bi 2 OS 2 / Nb...

Embodiment 2

[0031] Step 2. Slowly add 32g of p-bromophenol and 8g of chloropropene under vigorous stirring. At this time, the temperature is controlled at 50°C, and the reaction is refluxed at 80°C for 3h after the dropwise addition; the rest of the steps are the same as in Example 1.

Embodiment 3

[0033] Step 2. Slowly add 28g of p-bromophenol and 8g of chloropropene under vigorous stirring. At this time, the temperature is controlled at 50°C, and the reaction is refluxed at 80°C for 3h after the dropwise addition; the rest of the steps are the same as in Example 1.

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PUM

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Abstract

The invention discloses a synthesis method of 4-bromophenyl allyl ether. In the synthesis method, sodium bromide, anhydrous potassium carbonate, P-bromophenol, chloropropene, Nb2O5, K4Nb6O17, and thiourea are used as main raw materials; and P-bromophenol and chloropropene are subjected to substitution reaction under the action of a catalyst Bi2OS2 / Nb6O17-NH3. Compared with a conventional synthesismethod, in the method, a two-dimensional laminar composite catalyst is used in a multi-phase reaction system, so that the difficulty of the separation of the product catalyst and a problem of low yield caused by multiple side reactions are avoided, and further the yield of products is greatly increased and the purity of the products is greatly improved.

Description

technical field [0001] The invention relates to a method for synthesizing an intermediate p-bromophenyl allyl ether, belonging to the field of chemical synthesis. Background technique [0002] P-bromophenyl allyl ether can be used as pharmaceutical intermediates and active flame retardant diluents. With quaternary ammonium salt as a phase transfer catalyst, bromopropene and p-bromophenol are synthesized or acetone is used as solvent, bromopropene and p-bromophenol Bromophenol reaction to prepare p-bromophenyl allyl ether. However, the quaternary ammonium salt is not easy to separate from the organic phase, which affects the use of the product. The price of acetone and propylene bromide is also high. Generally, an anhydrous polar solvent and an appropriate amount of phase transfer catalyst can be used to obtain alkene with higher yield and purity. Propyl ether compound. If there is water in the polar solvent, the phenolic hydroxyl group and para-hydrogen will be directly re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C41/16C07C43/225
CPCC07C41/16B01J27/24C07C43/225
Inventor 杨程飞扬马素琴
Owner 杨程飞扬
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