Acetohydrazide → HCID 57650585, Verbindung

HRID 2063476Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2063476
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([NH:10][C:11]([C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=S)[CH3:9])=[CH:4][CH:3]=1.[C:25]([NH:28][NH2:29])(=O)[CH3:26]>C(#N)C.C([O-])(=O)C.[Hg+2].C([O-])(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([N:10]2[C:25]([CH3:26])=[N:28][N:29]=[C:11]2[C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH3:9])=[CH:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 14039AcetohydrazideHCID 57650584HCID 57650584, Verbindung

Produkt 1

HCID 57650585HCID 57650585, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 15337Mercuric acetateKatalysatorHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a mixture of the product of Step B (1.7 g, 4.6 mmol) and acetic hydrazide (0.76 g, 9.2 mmol) in 30 ml acetonitile was added mercury (II) acetate (2.2 g, 6.9 mmol) and the mixture was stirred at room temperature for overnight. The mixture was filtered over a Celite-fritted funnel and washed with more acetonitrile. The filtrate was concentrated in vacuo. Run wash column yield the desired product containing minor impurities (1.3 g, 72%), was used in the next step without further purification.

Aufarbeitung

  1. filtrationThe mixture was filtered over a Celite-fritted funnel
  2. washwashed with more acetonitrile
  3. concentrationThe filtrate was concentrated in vacuo
  4. washRun wash column

Quellen und Nachweise

ORD-Eintrag
ord-c239f37011df4052a4fc9114b05adc20
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288371B2

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