Reaktion #432385

Reaktionsgleichung

diethylene triamine

chloroformate

diethylenetriamine

→

product

Diethylene-triamine Carbamate

Lösungsmittel

hexane

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas removed
2. 2
   WaschenThe upper layer was washed twice with 3 l 5% aqueous sodium hydroxide
3. 3
   Sonstigephase separation
4. 4
   workup.ADDITIONwas assisted by the addition of salt, NaCl (to give brine in situ)
5. 5
   WaschenAfter a final wash with basic brine
6. 6
   Trocknenthe organic layer was dried (over Na2SO4 )
7. 7
   Filtrationfiltered

Vorschrift

A 988 g (1:04 mole) portion of polyisobutyl-24 chloroformate prepared according to the procedure outlined in Example 2, which had been diluted to 1800 ml with toluene was combined with 1800 ml of a solution containing 870 ml (8.05 moles) of diethylenetriamine in toluene using a Kenics static mixer (11 inches×3/8 inch); the reaction mixture was discharged into a 5 liter receiver. The reaction mixture was stripped, and then diluted with 8 1 hexane. A lower layer containing excess diethylene triamine was removed. The upper layer was washed twice with 3 l 5% aqueous sodium hydroxide; phase separation was assisted by the addition of salt, NaCl (to give brine in situ). After a final wash with basic brine, the organic layer was dried (over Na2SO4 ), filtered and stripped to give the above-identified product as a viscous yellow liquid (AV=64).

Quelle