Reaktion #310459

Reaktionsgleichung

dimethylaminopropylamine

hexamethylene diisocyanate

→

product

Ausbeute 59.3%

(CH3)2N(CH2)3NHCONH(CH2)6NHCONH(CH2)3N(CH3)2

Ausbeute 59.3%

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture is refluxed overnight, in the process of which crystals
2. 2
   Sonstigeprecipitate
3. 3
   FiltrationThe crystals are filtered with suction at room temperature
4. 4
   Waschenwashed with CH2Cl2
5. 5
   Sonstigedried
6. 6
   SonstigeRecrystallisation
7. 7
   workup.ADDITIONfrom a mixture of 1000 ml of acetone and 800 ml of ethanol

Vorschrift

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).

Quelle