Ammonium Hydroxide → 3-(Benzyl)benzamide

HRID 413827Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 413827
[CH2:1]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11](O)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(Cl)(=O)C(Cl)=O.[NH4+:23].[OH-]>CN(C=O)C.C(Cl)Cl>[CH2:1]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][CH:16]=1)[C:11]([NH2:23])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 3

HCID 14923Ammonium HydroxideHCID 65578Oxalyl chlorideHCID 41245533-Benzylbenzoic acid

Produkt 1

HCID 222388273-(Benzyl)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To the product from Step A (0.0119 moles) was added 150 mL of CH2Cl2, one drop of DMF, 10 mL of oxalyl chloride, and the mixture was stirred at room temperature for 3 hours. After cooling to 10° C., 30 mL of NH4OH (exothermic) was added and the mixture was stirred for 30 min. The reaction mixture was then concentrated and the resulting residue diluted with ethyl acetate. The organic layer was washed with 1N NaOH, brine, dried over Na2SO4, and concentrated to give the 3-(benzyl)benzamide as a white solid, which was used without further purification.

Aufarbeitung

  1. temperatureAfter cooling to 10° C.
  2. stirringthe mixture was stirred for 30 min
  3. concentrationThe reaction mixture was then concentrated
  4. additionthe resulting residue diluted with ethyl acetate
  5. washThe organic layer was washed with 1N NaOH, brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-14e0f63570d8410fba63ef985f301394
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06569851B1

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