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Hydrochloric Acid → HCID 19424596, Verbindung

HRID 743500
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 743500
[CH2:1]1[N:8]([CH2:9][CH2:10][NH+:11]([CH2:22][C:23]([O-:25])=[O:24])[CH2:12][CH2:13][N:14]2[CH2:21][C:19](=[O:20])[O:18][C:16](=[O:17])[CH2:15]2)[CH2:7][C:5](=[O:6])[O:4][C:2]1=[O:3].[NH2:26][CH2:27][CH2:28][CH2:29][CH2:30][NH2:31].Cl>CN(C=O)C.CN(C=O)C.C1CN2C(=NCCC2)C1>[C:16]([CH2:15][N:14]1[CH2:21][C:19](=[O:20])[NH:31][CH2:30][CH2:29][CH2:28][CH2:27][NH:26][C:2](=[O:3])[CH2:1][N:8]([CH2:7][C:5]([OH:6])=[O:4])[CH2:9][CH2:10][N:11]([CH2:22][C:23]([OH:25])=[O:24])[CH2:12][CH2:13]1)([OH:18])=[O:17]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 1045PutrescineHCID 16760401Diethylenetriaminepentaacetic dianhydride

Produkt 1

HCID 19424596HCID 19424596, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittel2×
HCID 131719551
HCID 131719551, Verbindung
Lösungsmittel

Versuchsvorschrift

A 1 L three-neck flask was charged with 340 mL of dry DMF. Two syringes were charged separately with solutions of diethylenetriaminepentaacetic acid dianhydride (3.00 g, 8.40 mmol) in 100 mL of DMF and 1,4-diaminobutane (0.740 g, 8.40 mmol) in DMF/DBN, (96 mL/4 mL). The solutions were added simultaneously at ambient temperature to the flask at a rate of 30 mL/hour. After the addition was complete, the reaction mixture was allowed to stir overnight, stripped to dryness, and 1N HCl added to adjust the pH to 10.4. The solution was applied to AG1-X8 (100-200 mesh, OAc-) resin and eluted with 0.5N acetic acid to yield 0.52 g (13.6%) as a white solid, after removal of acetic acid and lyophilization.

Aufarbeitung

  1. additionThe solutions were added simultaneously at ambient temperature to the flask at a rate of 30 mL/hour
  2. additionAfter the addition
  3. additionadded
  4. washeluted with 0.5N acetic acid
  5. customto yield 0.52 g (13.6%) as a white solid
  6. customafter removal of acetic acid and lyophilization

Quellen und Nachweise

ORD-Eintrag
ord-1dcdd200f8024a8398612ef6a82c7878
Quelldatensatz
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05556968

Notizen zur Reaktion

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