1-Azido-2-[2-(2-azidoethoxy)ethoxy]ethane → Bis-Aminoethylglycol

HRID 1451148Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1451148
[N:1]([CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11][N:12]=[N+]=[N-])=[N+]=[N-].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[NH2:1][CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11][NH2:12]

Komponenten

4

Edukt 2

HCID 108457051-Azido-2-[2-(2-azidoethoxy)ethoxy]ethaneHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 70248Bis-AminoethylglycolAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

The diazide (17) (3.55 g, 17.85 mmol) in THF (10 mL) was added dropwise into a cold (-5° C.) stirred mixture of lithium aluminum hydride (1.83 g, 48.2 mmol) in THF (20 mL). The reaction mixture was kept at -5° C. and carefully quenched with water (10 mL). The THF layer was filtered to remove the inorganic salts, dried over Na2SO4, and evaporated in vacuo to afford the diamine (18) (2.56 g, 97% yield).

Aufarbeitung

  1. customwas kept at -5° C.
  2. customcarefully quenched with water (10 mL)
  3. filtrationThe THF layer was filtered
  4. customto remove the inorganic salts
  5. dry with materialdried over Na2SO4
  6. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7f65df5ac9d149aea28e3e9ee7157ad3
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05604095

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