反应详情

(V-a): Propylene oxide (181.6 g, 0.3 mol) in 25 mL of absolute ethanol was added dropwise for 4.5 hours to a solution of N,N'-bis(2-hydroxypropyl)ethylenediamine (IV-a) (55 g, 0.3 mol) in 50 mL each of absolute ethanol, methanol and distilled water at 80° C. The reaction mixture was cooled and concentrated to give a milky white viscous suspension. The suspension was dissolved in ether and dried over anhydrous sodium sulfate. Unreacted (IV-a) precipitated and was removed by filtration. Ether was removed from the clear filtrate to produce a viscous liquid. Fractional distillation of the oil produced N,N,N'-tris(2-hydroxypropyl)ethylenediamine [bp. 140° C. at 0.15 mm; yield 55 percent; IR(neet): 3350(broad OH); NMR(CDCl3): δ 3.8(broad m, 3H); 2.5(broad m, 10H); 1.1(d, 9H)].

1. distillationdistilled water at 80° C
2. temperatureThe reaction mixture was cooled
3. concentrationconcentrated
4. customto give a milky white viscous suspension
5. dry with materialdried over anhydrous sodium sulfate
6. customUnreacted (IV-a) precipitated
7. customwas removed by filtration
8. customEther was removed from the clear filtrate
9. customto produce a viscous liquid
10. distillationFractional distillation of the oil