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

HRID 399367

Reaktionsgleichung

Reaktionsgleichung von HRID 399367
[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 the reaction is completed, 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 out and dried.

Aufarbeitung

  1. concentrationconcentration
  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 out
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b8b16aaaca1e4eaeb10499e1d4ff9603
Quelldatensatz
uspto-grants-1998_10
Patentnummer
US05820849

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