Diethyl 2-(((4-Chlorobenzyl)amino)carbonyl)malonate → HCID 178522947, Verbindung

HRID 411187

Reaktionsgleichung

Reaktionsgleichung von HRID 411187
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]([CH2:6][NH:7][C:8]([CH:10]([C:16]([O:18]CC)=O)[C:11]([O:13]CC)=O)=[O:9])=[CH:4][CH:3]=1.[N:23]1([CH2:29][C:30]2[S:34][C:33]([NH2:35])=[N:32][N:31]=2)[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>C1(C)C(C)=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:11](=[O:13])[N:35]=[C:33]3[S:34][C:30]([CH2:29][N:23]4[CH2:28][CH2:27][O:26][CH2:25][CH2:24]4)=[N:31][N:32]3[C:16]=2[OH:18])=[O:9])=[CH:21][CH:22]=1

Komponenten

4

Edukt 2

HCID 22397146Diethyl 2-(((4-Chlorobenzyl)amino)carbonyl)malonateHCID 223971795-(4-Morpholinylmethyl)-1,3,4-thiadiazol-2-ylamine

Produkt 1

HCID 178522947HCID 178522947, VerbindungAusbeute 39,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

Diethyl 2-(((4-chlorobenzyl)amino)carbonyl)malonate (Preparation 5, 33 mg) and 5-(4-morpholinylmethyl)-1,3,4-thiadiazol-2-ylamine (Preparation 4, 20 mg) are dissolved in xylene and heated to reflux for 5 h. The solvent is evaporated and the residue is triturated with ether. The resulting percipitate is filtered and dried to afford 17 mg of the title compound as a brown solid. Physical characteristics: MS (ESI+) m/z 438 (M+H)+. 1H NMR (DMSO) δ 7.42, 7.38, 4.60, 3.92, 3.62, 2.62.

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux for 5 h
  3. customThe solvent is evaporated
  4. customthe residue is triturated with ether
  5. filtrationThe resulting percipitate is filtered
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-5ec67ceeffca4ca98ac05e7d972b9036
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06559145B2

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