Acetic Acid → HCID 86722263, Verbindung

HRID 869417Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 869417
[NH2:1][C:2]1[C:6]2[C:7]([Br:13])=[C:8]([O:11][CH3:12])[CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:14](=[O:28])[CH:15]=[CH:16][C:17]1[N:18]=[C:19]([NH:22][C:23](=[O:27])[CH:24]([CH3:26])[CH3:25])[S:20][CH:21]=1.CC#N.CC(O)=O.OP(O)(O)=O>[Cl-].[Cl-].[Zn+2].O>[Br:13][C:7]1[C:6]2[C:2]3[NH:1][CH:16]([C:17]4[N:18]=[C:19]([NH:22][C:23](=[O:27])[CH:24]([CH3:26])[CH3:25])[S:20][CH:21]=4)[CH2:15][C:14](=[O:28])[C:3]=3[O:4][C:5]=2[CH:10]=[CH:9][C:8]=1[O:11][CH3:12]

Komponenten

7

Edukt 4

HCID 176Acetic AcidHCID 1004Phosphoric AcidHCID 6342AcetonitrileHCID 86722262HCID 86722262, Verbindung

Produkt 1

HCID 86722263HCID 86722263, VerbindungAusbeute 55,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3007855ZincchlorideKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A mixture of 16A (2 g, 4.3 mmol), ZnCl2 (6 g), MeCN (10 mL), AcOH (2 mL) and H3PO4 (2 mL) was heated to 90° C. and reacted overnight. TLC monitored the reaction. After the reaction completed, the reaction mixture was added dropwise into water, extracted with ethyl acetate and concentrated to give 16B (1.1 g, 55% yield).

Aufarbeitung

  1. customreacted overnight
  2. customthe reaction
  3. extractionextracted with ethyl acetate
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-7357f5891e964d5ab3ca22ae9acd37d7
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969373B2

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