Synthesis
255.7 g of formic acid (equivalent to 38.3 g of water) and 99% pure diisopropylamine (460 g, 85% pure) were added to a 1 L autoclave, and stirring was initiated to ensure the formation of a homogeneous reaction system. The molar ratio of formic acid to diisopropylamine was controlled to be 1.05:1. Under continuous stirring, the reaction system was heated to about 200 °C, at which time the pressure in the autoclave was increased to about 1.7 MPa and stabilized, and the reaction conditions were maintained for about 3 hours. Upon completion of the reaction, the pressure in the autoclave was slowly released. Subsequently, carbon monoxide and water vapor generated during the reaction were collected and the reaction products were separated, resulting in about 709 g of a homogeneous and transparent N,N-diisopropylformamide solution.
References
[1] Research on Chemical Intermediates, 2013, vol. 39, # 6, p. 2843 - 2848
[2] Comptes Rendus Chimie, 2012, vol. 15, # 11-12, p. 980 - 987
[3] Bulletin of the Korean Chemical Society, 2010, vol. 31, # 10, p. 2989 - 2991
[4] Synlett, 2010, # 8, p. 1231 - 1234
[5] Synlett, 2010, # 14, p. 2093 - 2096
