反应详情

温度

90 °C

To a large excess of 1,4-diaminobutane (85 g, 0.964 mol) at 90° C. under argon was slowly added (over 2 hours) B2 (10.50 g, 0.030 mol). The solution was heated at 90° C. overnight and the excess diamine distilled off under reduced pressure (0.1 mbar, 28° C.) to quantitatively yield the title compound as a pale yellow low melting point solid: C24H42N4O3 requires 434. Found DCl: M+ +1 435. I.R. 1664 cm−1 (CO2). δH (CDCl3) 1.15-1.40 (10H, br m, (CH2)3CH2CH, NH2), 1.40-1.60 (10H, br m, (CH2)2CH2NH2, CH2CH2O), 1.76 (2H, q, CH2CH), 2.63 (4H, t, CH2NH2), 2.93 (2H, t, CH2CH), 3.16 (4H, q, CH2NH), 3.37. (2H, t, CH2OCH2Ph), 4.42 (2H, s, CH2Ph), 7.26 (5H, m, Ph), 7.61 (2H, t, CONH). δC (CDCl3) 25.7 (1C, CH2(CH2)2CH), 26.6 (2C, CH2CH2NH2), 28.8, 29.4 (2C, CH2CH2CH, CH2CH2O), 30.6 (2C, CH2CH2NH), 32.7 (1C, CH2CH), 39.0 (2C, CH2NHCO), 41.4 (2C, CH2NH2), 54.7 (1C, CHCO), 70.1, 72.6 (2C, CH2OCH2), 127.2 (1C, CH(CH)2C), 127.3 (2C, CHC), 128.0 (2C, CHCHC), 138.5 (1C, CCH2O), 171.0 (2C, CONH).

1. distillationthe excess diamine distilled off under reduced pressure (0.1 mbar, 28° C.)