Hydrochloric Acid → 3-Ethynylbenzonitrile

HRID 606787

Reaktionsgleichung

Reaktionsgleichung von HRID 606787
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[C:16]#[N:17])(C)C.Cl>CO>[C:12]([C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[C:16]#[N:17])#[CH:11]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 225703183-[(Trimethylsilyl)ethynyl]benzonitrile

Produkt 1

HCID 120889643-EthynylbenzonitrileAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Add potassium carbonate (0.138 g, 1 mmol) to a solution of 3-trimethylsilanylethynylbenzonitrile from PREPARATION 5 (2.0 g, 10.1 mmol) in methanol (50 mL). Stir the mixture at room temperature for 20 min and add a 10% aqueous hydrochloric acid solution (4 mL). Concentrate to a reduced volume, add diethyl ether and water and separate the phases. Wash once the aqueous phase with diethyl ether. Combine the organic phases, dry over sodium sulfate and concentrate to obtain the title compound as a solid (1.17 g, 92%).

Aufarbeitung

  1. concentrationConcentrate to a reduced volume
  2. additionadd diethyl ether and water
  3. customseparate the phases
  4. washWash once the aqueous phase with diethyl ether
  5. dry with materialdry over sodium sulfate
  6. concentrationconcentrate

Quellen und Nachweise

ORD-Eintrag
ord-0eabd544b1254993971a164e6b861429
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07915424B2

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