反应详情

302.4 g (1.2 mol) carbonyl-bis-caprolactam was dissolved in 400 ml ethyl acetate at 78° C. In one hour 69.3 g (0.4 mol) triamino nonane, dissolved in 100 ml ethyl acetate, was added dropwise. The reaction was monitored by means of TLC. After 3 hours the clear solution was cooled to room temperature and extracted 4 times with 500 ml water (with some NaCl). The solution was then dried with NaSO4. The NaSO4 was removed by filtration and the ethyl acetate was removed by means of the rotavapor. The product was dried at 75° C. and in a vacuum. Caprolactam-blocked of 1,8-diisocyanato, 4-(isocyanatomethyl) nonane was obtained pure, as a lightly coloured oil (yield=99%).

1. additionwas added dropwise
2. extractionextracted 4 times with 500 ml water (with some NaCl)
3. dry with materialThe solution was then dried with NaSO4
4. customThe NaSO4 was removed by filtration
5. customthe ethyl acetate was removed by means of the rotavapor
6. customThe product was dried at 75° C. and in a vacuum