Hydrochloric Acid → HCID 12398997, Verbindung

HRID 2301261Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2301261
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH:10](Br)[CH3:11])=[CH:5][CH:4]=1.[CH3:14][O:15][C:16]1[CH:21]=C[C:19](OC)=[CH:18][CH:17]=1.C[N:25](C)C1C=CC=CC=1.Cl>>[CH3:14][O:15][C:16]1[CH:21]=[C:11]2[C:19](=[CH:18][CH:17]=1)[NH:25][C:9]([C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)=[CH:10]2

Komponenten

5

Versuchsvorschrift

A solution of p-methoxy-2-bromopropiophenone ((1 g, 4.11 mmol) was added to a solution of p-methoxyanisole in N,N dimethylaniline (1.7 g, 13.82 mmol)) and heated under reflux for 3 hours. The reaction mixture was cooled to room temperature, poured into 2N HCl, and extracted with EtOAc. The organic extract was washed with water and dried over Na2SO4. Removal of the solvent under reduced pressure and flash chromatography on SiO2 using CH2Cl2 gave the desired intermediate compound 2.

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. extractionextracted with EtOAc
  4. extractionThe organic extract
  5. washwas washed with water
  6. dry with materialdried over Na2SO4
  7. customRemoval of the solvent under reduced pressure and flash chromatography on SiO2

Quellen und Nachweise

ORD-Eintrag
ord-3def2fc80867488f818c85d12d1174e2
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06500669B1

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