反应详情

204.3 g of dimethylaminopropylamine are added dropwise to a solution of 168.2 g of hexamethylene diisocyanate in 100 ml of methylene chloride and the mixture is refluxed overnight, in the process of which crystals precipitate. The crystals are filtered with suction at room temperature, washed with CH2Cl2 and dried. Recrystallisation from a mixture of 1000 ml of acetone and 800 ml of ethanol yields 221.0 g (59.3%) of product with a melting point of 159° C. Tritration: 2 equivalents=376.7 g (theory 372.6 g).

1. temperaturethe mixture is refluxed overnight, in the process of which crystals
2. customprecipitate
3. filtrationThe crystals are filtered with suction at room temperature
4. washwashed with CH2Cl2
5. customdried
6. customRecrystallisation
7. additionfrom a mixture of 1000 ml of acetone and 800 ml of ethanol