Diethylenetriamine → N,N''-Di-Z-diethylenetriamine

HRID 1067173

Reaktionsgleichung

Reaktionsgleichung von HRID 1067173
[NH2:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH2:7].C(N([CH2:13][CH3:14])CC)C.C([C:17]([O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:18])#N>ClCCl>[CH2:20]([O:19][C:17]([NH:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][C:17]([O:19][CH2:20][C:14]1[CH:13]=[CH:23][CH:22]=[CH:21][CH:26]=1)=[O:18])=[O:18])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

Komponenten

5

Edukt 3

HCID 8111DiethylenetriamineHCID 8471TriethylamineHCID 79660Benzyl cyanoformate

Produkt 1

HCID 4367374N,N''-Di-Z-diethylenetriamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

51.5 g (500 mmol) of diethylenetriamine and 139 ml (1 mol) of triethylamine are dissolved in dichloromethane and mixed at −20° C. with 161 g of benzyl cyanoformate (Fluka) in dichloromethane and then stirred overnight at room temperature. After completion of the reaction, concentration by evaporation is performed during draw-off, the residue is taken up in diethyl ether, the organic phase is washed with sodium carbonate solution and dried with sodium sulfate. The filtrate is mixed with hexane, the precipitate is filtered off and dried.

Aufarbeitung

  1. customAfter completion of the reaction, concentration
  2. customby evaporation
  3. washthe organic phase is washed with sodium carbonate solution
  4. dry with materialdried with sodium sulfate
  5. additionThe filtrate is mixed with hexane
  6. filtrationthe precipitate is filtered off
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a661f4bf15364d70800b20b465097663
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06248306B1

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