Реакция #310459

Уравнение реакции

dimethylaminopropylamine

hexamethylene diisocyanate

→

product

Выход 59.3%

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

Выход 59.3%

Растворители

methylene chloride

Условия реакции

Обработка

1. 1
   Температураthe mixture is refluxed overnight, in the process of which crystals
2. 2
   Другоеprecipitate
3. 3
   ФильтрацияThe crystals are filtered with suction at room temperature
4. 4
   Промывкаwashed with CH2Cl2
5. 5
   Другоеdried
6. 6
   ДругоеRecrystallisation
7. 7
   workup.ADDITIONfrom a mixture of 1000 ml of acetone and 800 ml of ethanol

Методика

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).

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