Synthesis
The general procedure for the synthesis of 2,2'-diaminoethylene glycol diphenyl ether from 1,2-bis(2-nitrophenoxy)ethane was as follows: 60 g of 1,2-bis(2-nitrophenoxy)ethane, 51.7 g of sodium hydrosulfide solution with a mass fraction of 26% and 120 g of water were added to a 1 L autoclave. After replacing the air in the kettle with nitrogen, stirring was initiated and the reaction was heated to 130 °C, the reaction pressure was maintained at 0.2 MPa, and the reaction was held for 5 h. After completion of the reaction, the pressure was slowly released and cooled to 30~35 °C, followed by filtration to collect the crude product. The crude product was dissolved in 300 ml of water and acidified with hydrochloric acid. After drying, 44.4 g of the target product 2,2'-diaminoethylene glycol diphenyl ether was finally obtained in 91.0% yield and 99.65% purity.
References
[1] Zeitschrift fuer Naturforschung, B: Chemical Sciences, 1992, vol. 47, # 4, p. 547 - 552
[2] Chemistry of Heterocyclic Compounds (New York, NY, United States), 1988, vol. 24, p. 106 - 109
[3] Khimiya Geterotsiklicheskikh Soedinenii, 1988, vol. 24, # 1, p. 126 - 130
[4] Patent: CN105884631, 2016, A. Location in patent: Paragraph 0023; 0024
[5] Inorganic Chemistry, 2015, vol. 54, # 8, p. 3929 - 3936
