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Ethyl Acetate → HCID 67072706, Verbindung

HRID 386553
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 386553
Cl[C:2]1[C:7](C2C=CC=CC=2)=[N:6][NH:5][C:4](=[O:14])[CH:3]=1.[C:15]([O-])([O-])=[O:16].[K+].[K+].Br[CH2:22][C:23]1[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=1.CCOC(C)=O>CN(C=O)C.[Cl-].[Na+].O>[CH3:15][O:16][C:2]1[CH:7]=[N:6][N:5]([CH2:22][C:23]2[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=2)[C:4](=[O:14])[CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 1650214-Methoxybenzyl bromideHCID 27358035-Chloro-6-phenylpyridazin-3-ol

Produkt 1

HCID 67072706HCID 67072706, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228
Dimethylformamide
Lösungsmittel
HCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

To a stirring solution of 5-chloro-6-phenylpyridazin-3(2H)-one (78 mg, 0.618 mmol) in DMF (3 mL) at room temperature under argon was added K2CO3 (256 mg, 1.855 mmol), and was followed by addition of 1-(bromomethyl)-4-methoxybenzene (149 mg, 0.742 mmol). The resulting reaction mixture was stirred at room temperature overnight. EtOAc (20 mL) and brine (30 mL) were added to the reaction mixture. Layers were separated. Organic layer were washed with water (15 mL), and brine (15 mL). Organic phase was dried (MgSO4), filtered and concentrated. Crude product (117 mg) (MS (ESI) 247 (M+H)) was used directly to next step.

Aufarbeitung

  1. customThe resulting reaction mixture
  2. customLayers were separated
  3. washOrganic layer were washed with water (15 mL), and brine (15 mL)
  4. dry with materialOrganic phase was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-2ddd7232a5654c34a71000a89eb967de
Quelldatensatz
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08372837B2

Notizen zur Reaktion

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