Hydrogen Peroxide → HCID 44236488, Verbindung

HRID 1503186Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1503186
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][C:7]([CH3:12])([CH3:11])[CH2:8][C:9]#[N:10])=[CH:4][CH:3]=1.OO.C(=O)([O-])[O-:18].[K+].[K+].O>CS(C)=O.C(Cl)Cl>[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][C:7]([CH3:11])([CH3:12])[CH2:8][C:9]([NH2:10])=[O:18])=[CH:4][CH:3]=1

Komponenten

7

Edukt 4

HCID 784Hydrogen PeroxideHCID 962WaterHCID 11430Potassium CarbonateHCID 58155372HCID 58155372, Verbindung

Produkt 1

HCID 44236488HCID 44236488, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 3-(4-chlorophenoxy)-3-methylbutyronitrile (60.4 mmol) in DMSO (75 mL) is treated with H2O2 (50% w/w) (434 mmol) and potassium carbonate (121 mmol) at zero degrees Celsius. The reaction mixture is stirred at room temperature over the weekend. The reaction mixture is transferred into a separatory funnel using water (100 mL) and CH2Cl2 (200 mL). The mixture is equilibrated and the CH2Cl2 layer is removed. The aqueous layer is extracted two additional times with CH2Cl2 (2×300 mL). The combined CH2Cl2 extracts are washed 5 consecutive times with water (5×200 mL) followed by a brine (500 mL) wash, dried over anhydrous MgSO4, filtered, and concentrated under reduced pressure, which affords 3-(4-chlorophenoxy)-3-methylbutyramide.

Aufarbeitung

  1. customThe reaction mixture is transferred into a separatory funnel
  2. customthe CH2Cl2 layer is removed
  3. extractionThe aqueous layer is extracted two additional times with CH2Cl2 (2×300 mL)
  4. washThe combined CH2Cl2 extracts are washed 5 consecutive times with water (5×200 mL)
  5. washwash
  6. dry with materialdried over anhydrous MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure, which

Quellen und Nachweise

ORD-Eintrag
ord-31e73f921b11401c826b3d5c56ed38a9
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09212155B2

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