5-Amino-o-cresol synthesis
- Product Name:5-Amino-o-cresol
- CAS Number:2835-95-2
- Molecular formula:C7H9NO
- Molecular Weight:123.15
95-74-9
2835-95-2
General procedure for the synthesis of 2-methyl-5-aminophenol from 3-chloro-4-methylaniline: 1700 kg of 50% sodium hydroxide solution was added to a 4800 L autoclave, followed by 1850 kg of ethanol solution containing 1000 kg of 3-chloro-4-methylaniline. Then 50kg of cuprous chloride and 15kg of copper powder were added as catalyst. The reaction vessel was sealed and replaced with nitrogen five times to ensure an oxygen-free environment. The reaction mixture was heated to 175°C and maintained at this temperature for 4 hours, during which time it was sampled and analyzed to monitor the progress of the reaction. Upon completion of the reaction, the mixture was cooled to room temperature. Ethanol was recovered under reduced pressure and then the reaction mixture was filtered and transferred to an 8000 L tank. The pH was adjusted to weak acidity by adding 1450 kg of industrial hydrochloric acid to the filtrate. Extraction was carried out with 2000L of ethyl acetate for three times. The organic phases were combined and the ethyl acetate was recovered by distillation under reduced pressure to obtain the crude product. To the crude product, 1000kg of ethanol was added, heated to 60°C to dissolve, and then 50kg of activated carbon was added to decolorize. After stirring for 1 hour, the activated carbon was removed by hot filtration and the filtrate was cooled to 5°C for crystallization. Finally, 707kg of 2-methyl-5-aminophenol was obtained with a yield of 85.36% and a purity of 99.8%.
95-74-9
250 suppliers
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2835-95-2
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$8.00/25g
Yield:2835-95-2 85.36%
Reaction Conditions:
with copper;copper(l) chloride;sodium hydroxide in ethanol at 175; for 4 h;Autoclave;Inert atmosphere;Industrial scale;Reagent/catalyst;
Steps:
1 Example 1
In a 4800L autoclave, 1700 kg of 50% sodium hydroxide solution was added, 1850 kg of an ethanol solution containing 1000 kg of 3-chloro-4-methylaniline was added, 50 kg of cuprous chloride and 15 kg of copper powder were added, and the reaction vessel was sealed and replaced with nitrogen 5 times. Warm up to 175°C, incubate for 4 hours, sample and analyze. After passing the test, cool down. Ethanol is recovered under reduced pressure, filtered into an 8000L tank, neutralized by adding 1450 kg of industrial hydrochloric acid to weak acidity, extracted with 2000 L of ethyl acetate and extracted three times, and ethyl acetate is recovered under reduced pressure. , get crude. The crude product was added with 1000 kg of ethanol, heated to 60° C., and 50 kg of activated carbon was added. After stirring for 1 hour, the mixture was filtered and cooled to 5° C. to obtain 707 kg of a product with a yield of 85.36% and a purity of 99.8%.
References:
Zhejiang Dinglong Technology Co., Ltd.;Pan Zhijun;Ye Jiongying;Jin Ningren;Xu Huigang;Zhang Xue CN107963974, 2018, A Location in patent:Paragraph 0030-0032; 0036; 0037
5428-54-6
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2835-95-2
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106-49-0
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2835-95-2
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99-55-8
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2835-95-2
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2835-95-2
430 suppliers
$8.00/25g