1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 19848625, Verbindung

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Reaktionsgleichung

[NH2:1][CH2:2][CH:3]1[O:8][CH:7]([CH3:9])[CH2:6][N:5]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])[CH2:4]1.[NH2:18][C:19]1[C:27]([Cl:28])=[CH:26][C:22]([C:23](O)=[O:24])=[C:21]([O:29][CH2:30][CH3:31])[CH:20]=1.Cl.C(N=C=NCCCN(C)C)C>ClCCl>[NH2:18][C:19]1[C:27]([Cl:28])=[CH:26][C:22]([C:23]([NH:1][CH2:2][CH:3]2[O:8][CH:7]([CH3:9])[CH2:6][N:5]([CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[CH2:4]2)=[O:24])=[C:21]([O:29][CH2:30][CH3:31])[CH:20]=1

Komponenten

Reaktionsbedingungen

Temperatur: 25 °C

Versuchsvorschrift

To a solution of 2-aminomethyl-4-(2-chlorobenzyl)-6-methylmorpholine (2.2 g) in dichloromethane (50 ml), 4-amino-5-chloro-2-ethoxybenzoic acid (1.9 g) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.7 g) are added. The reaction mixture is stirred at 25° C. for 4 hours, washed successively with water, aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The solvent is distilled off under reduced pressure, and the residue is chromatographed on silica gel with ethyl acetate-hexanechloroform (1:1:1) to give the title compound (2.6 g) as an oil.

Aufarbeitung

washwashed successively with water, aqueous sodium hydroxide solution and saturated aqueous sodium chloride solution
dry with materialdried over magnesium sulfate
distillationThe solvent is distilled off under reduced pressure
customthe residue is chromatographed on silica gel with ethyl acetate-hexanechloroform (1:1:1)

Quellen und Nachweise

ORD-Eintrag: ord-95de7eb35e774e099fd55593746543c0
Quelldatensatz: uspto-grants-1989_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04870074

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