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Dimethylformamide → HCID 13175316, Verbindung

HRID 2418216
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2418216
CN(C)C=O.Cl[C:7]([O:9][CH2:10][CH3:11])=[O:8].[O:12]=[C:13]1[N:18]2[C:19]3[C:24]([NH:25][CH2:26][C:17]2=[N:16][CH:15]=[C:14]1[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:23][CH:22]=[CH:21][CH:20]=3>O>[O:12]=[C:13]1[N:18]2[C:19]3[C:24]([N:25]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:26][C:17]2=[N:16][CH:15]=[C:14]1[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[CH:23][CH:22]=[CH:21][CH:20]=3
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 10928Ethyl chloroformateHCID 13175315HCID 13175315, Verbindung

Produkt 1

HCID 13175316HCID 13175316, VerbindungAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

4 ml of dry dimethylformamide were saturated with nitrogen for 10 minutes before 150 mg of ethyl chloroformate and 280 mg of ethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2-carboxylate were added thereto. The solution obtained was left at room temperature overnight and then was poured into water. The mixture was extracted with ethyl acetate and the organic phase was dried over MgSO4 and evaporated to dryness. The residue was chromatographed over silica gel and eluted with ethyl acetate to obtain 140 mg (41% yield) of diethyl 5,6-dihydro-1-oxo-1H-pyrimido [1,2-a] quinoxaline-2,6-dicarboxylate melting at 140°-2° C.

Aufarbeitung

  1. additionwere added
  2. customThe solution obtained
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe organic phase was dried over MgSO4
  5. customevaporated to dryness
  6. customThe residue was chromatographed over silica gel
  7. washeluted with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-a24dfdf9a5314ed18eb735361453d567
Quelldatensatz
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04472401

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