Acetic Acid → HCID 86722256, Verbindung

HRID 869410Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 869410
[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:25])/[CH:15]=[CH:16]/[C:17]1[S:21][C:20]([CH:22]([CH3:24])[CH3:23])=[N:19][CH:18]=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[S:21][C:20]([CH:22]([CH3:23])[CH3:24])=[N:19][CH:18]=4)[CH2:15][C:14](=[O:25])[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 86722255HCID 86722255, Verbindung

Produkt 1

HCID 86722256HCID 86722256, VerbindungAusbeute 79,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3007855ZincchlorideKatalysatorHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A mixture of 14A (1.4 g, 3.3 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 14B (1.1 g, 78% yield).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-825a036e6540422db76d5b7a45e2bd17
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969373B2

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