3-Diethylaminophenol synthesis
- Product Name:3-Diethylaminophenol
- CAS Number:91-68-9
- Molecular formula:C10H15NO
- Molecular Weight:165.23
109-89-7
108-46-3
91-68-9
The general procedure for the synthesis of 3-hydroxy-N,N-diethylaniline from diethylamine and resorcinol is as follows: a Raney Ni-catalyzed amination of resorcinol with secondary amines was used. The procedure was as follows: resorcinol (2.2 g, 20 mmol), diethylamine (30 mmol) and Raney Ni catalyst (110 mg) were added to a 100 ml autoclave, and 50 ml of water was added as solvent. The air in the autoclave was replaced with hydrogen three times, followed by maintaining the hydrogen pressure at 0.05 MPa. The reaction mixture was rapidly heated to 200 °C and the reaction was stirred at this temperature for 3 h. The reaction was carried out at a temperature of 0.05 °C. After completion of the reaction, the mixture was cooled to room temperature and extracted with n-butyl acetate. The organic layer was collected, dried with anhydrous magnesium sulfate, filtered and concentrated to obtain the crude product. Finally, the target product 3-hydroxy-N,N-diethylaniline was purified by silica gel fast column chromatography (eluent was petroleum ether/ethyl acetate, 3:1, v/v).
Yield:91-68-9 98.5%
Reaction Conditions:
with sodium amide at 5; for 0.583333 h;
Steps:
2-6 One-step synthesis of m-diethylaminophenol
In a 500ml flask, add 200g of diethylamine, add 10g of catalyst sodium amide and 5g of super-base catalyst, stir and cool to 5°C, dropwise add 15g o-chlorophenol in 15 minutes. Turn on the ultrasonic, the ultrasonic frequency is 40kHz, the ultrasonic power is 100w, the temperature is raised to the diethylamine reflux state, the reaction is 20 minutes, and the reaction is over. Recycle diethylamine by rotary evaporation, add 60g of toluene, add 75g of water dropwise to quench the reaction when the temperature is below 5, add dropwise 5% hydrochloric acid aqueous solution to adjust pH=7, separate, wash with water, separate the liquid, rotate the organic phase to obtain the product The m-diethylaminophenol is 18.9 g, the yield is 98.5%, and the purity is 99.1%.
References:
Anhui Green Gu Chuangke Space Co., Ltd.;Li Fujia;Li Yunzheng;Wan Yuqing CN112142607, 2020, A Location in patent:Paragraph 0016-0020
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