Oxalyl chloride → HCID 71556276, Verbindung

HRID 929489Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 929489
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[C:10](O)[C:9]2=[O:21])=[CH:4][CH:3]=1.C(Cl)(=O)C([Cl:25])=O>CN(C=O)C>[Cl:25][C:10]1[C:9](=[O:21])[N:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[C:12](=[O:13])[C:11]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

4

Edukt 2

HCID 65578Oxalyl chlorideHCID 86709896HCID 86709896, Verbindung

Produkt 1

HCID 71556276HCID 71556276, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

After dissolving compound 6d (1.00 g, 3.33 mmol) in MC (10 ml) and anhydrous DMF (10 ml), oxalyl chloride (0.850 g, 6.66 mmoL) was added thereto and the agitation for 30 minutes was carried out. After the identification of the reaction progress with TLC, the reaction was terminated. Then, three times extractions were carried out with EA and three times washings were carried out with brine. Water was removed by using Na2SO4, solvents were removed and then, the column chromatography was carried out with EA/HX ( 1/15). The suspension was carried out with HX to obtain compound 7d.

Aufarbeitung

  1. additionwas added
  2. customAfter the identification of the reaction progress with TLC, the reaction was terminated
  3. extractionThen, three times extractions
  4. customWater was removed
  5. customwere removed

Quellen und Nachweise

ORD-Eintrag
ord-9a277de1c5bf4ac781df43b75492ee22
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09296690B2

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