Hydrochloric Acid → HCID 10261437, Verbindung

HRID 2116668Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2116668
[CH3:1][CH:2]([C:5]#[N:6])[C:3]#[N:4].Br[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].C(=O)([O-])[O-].[K+].[K+].Cl>CS(C)=O>[CH2:12]([O:11][C:9]([CH2:8][C:2]([CH3:1])([C:5]#[N:6])[C:3]#[N:4])=[O:10])[CH3:13]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 194252-Methylpropanedinitrile

Produkt 1

HCID 10261437HCID 10261437, VerbindungAusbeute 24,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

2.0 g of 2-methylmalononitrile and 4.2 g of ethyl bromoacetate were dissolved in 10 ml of dimethyl sulfoxide. 3.4 g of potassium carbonate was added thereto and stirred for 4 hours at room temperature. Then, to the reaction mixture was added dilute hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was subjected to silica gel column chromatography to give 1.0 g of 2-(ethoxycarbonylmethyl)-2-methylmalononitrile (hereinafter referred to as the present invention compound (74)).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed successively with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue obtained

Quellen und Nachweise

ORD-Eintrag
ord-6bfe6cba5082434ea2e3f139004d1f58
Quelldatensatz
uspto-grants-2008_10
Patentnummer
US07439266B2

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