4-PHENOXYBENZOIC ACID synthesis
- Product Name:4-PHENOXYBENZOIC ACID
- CAS Number:2215-77-2
- Molecular formula:C13H10O3
- Molecular Weight:214.22
Yield:2215-77-2 89%
Reaction Conditions:
Stage #1:phenol with sodium hydroxide in water at 60; for 2 h;
Stage #2:para-chlorobenzoic acid in tetralin at 150; for 10 h;Temperature;
Steps:
1-3 Example 2:
A new process for the synthesis of 4-phenoxybenzoic acid. The process is as follows: In a 250ml flask, add 94.6g of phenol, 78g of sodium hydroxide, and 70g of water, heat to 60 ° C, and react for 2 hours.Measure until the phenol is almost completely reacted to sodium phenate, keep the temperature until use;In a 1000 ml four-necked flask, 530 g of tetrahydronaphthalene and 158.7 g of p-chlorobenzoic acid were added, and a reflux water separation device was added to the system.The temperature is heated to about 150C, and a step of sodium phenol solution is slowly added dropwise. As the dropwise addition proceeds, the water separator will graduallyWater is distilled off, and the dropwise addition is completed in about 8 hours. After the dropwise addition, the reaction is held for 2 hours. After sampling, the test is performed.Should end. After the reaction was completed, the temperature was lowered to 30 ° C, and the obtained solid was added to a 1000 ml flask and stirred with 500 ml of water.After being washed with a mixture of pulp and filtered, the mixture was beaten with 300 ml of water and adjusted to pH 1 with concentrated hydrochloric acid. The crude 4-phenoxybenzoic acid was obtained by filtration.Wet product 318g. The above crude wet product was added to a 1000 ml flask, 600 g of 95% ethanol was added, and the mixture was heated to reflux until all the solids were dissolved.Then, slightly cool, add 5g of activated carbon, heat to reflux for 1h, filter while hot, and slowly reduce the obtained filtrate to 10C with stirring.In the following, a large amount of white solids were precipitated, filtered and dried to obtain 190.7 g of a dry product, with a purity of 99.5% and a yield of 89.0%.
References:
Chengwu Chenhui Environmental Protection Technology Co., Ltd.;Chen Hongping;Cui Lilong;Li Shoufeng CN110407693, 2019, A Location in patent:Paragraph 0015-0020
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