Sodium Bicarbonate → HCID 59557741, Verbindung

HRID 2403721Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2403721
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([CH:16]=1)[CH2:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=O)=[CH:10][CH:9]=1.[C:18]([O-])(O)=O.[Na+]>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([CH2:7][C:8]2[CH:15]=[CH:14][C:11]([CH:12]=[CH2:18])=[CH:10][CH:9]=2)[CH:16]=1

Komponenten

4

Edukt 2

HCID 516892Sodium BicarbonateHCID 59557754HCID 59557754, Verbindung

Produkt 1

HCID 59557741HCID 59557741, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

To a solution of Ph3PCH3I (0.97 g) in toluene (5 mL), KN(TMS)2 (0.5M in toluene, 4.8 mL) was added dropwise at room temperature. After 10 min, the solution of 4-(5-bromo-2-chlorobenzyl)benzaldehyde (intermediate AL) (0.62 g) in toluene (2 mL) was added dropwise. After 2 h, aqueous NaHCO3 was added to quench the reaction, and the resulting mixture was extracted with ethyl acetate. The organic layers were combined, washed with brine, and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the product was purified by column chromatography to obtain pure intermediate AM (0.5 g).

Aufarbeitung

  1. waitAfter 2 h
  2. customto quench
  3. customthe reaction
  4. extractionthe resulting mixture was extracted with ethyl acetate
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. customThe solvent was evaporated under reduced pressure
  8. customthe product was purified by column chromatography
  9. customto obtain pure intermediate

Quellen und Nachweise

ORD-Eintrag
ord-68f72d35eb7a4362bf15190ff00dec0f
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08802637B2

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