Sodium → HCID 13770583, Verbindung

HRID 236227Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 236227
[Na].Cl[CH2:3][CH2:4][CH:5]([CH3:20])[C:6]([NH:8][C:9]1[S:10][CH:11]=[C:12]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:13]=1[C:14]#[N:15])=[O:7]>C(O)C>[C:14]([C:13]1[C:12]([C:16]([CH3:19])([CH3:18])[CH3:17])=[CH:11][S:10][C:9]=1[N:8]1[CH2:3][CH2:4][CH:5]([CH3:20])[C:6]1=[O:7])#[N:15]

Komponenten

4

Versuchsvorschrift

To a solution of 0.21 g of sodium dissolved in 10 ml of ethanol was added 2.75 g of 4-chloro-N-[3-cyano-4-(1,1-dimethylethyl)-2-thienyl]-2-methylbutanamide dissolved in 35 ml ethanol dropwise. The mixture was allowed to stir at room temperature for about one hour and the solvent was removed in vacuo. The residue was combined with 10 ml ethanol and 250 ml water and the precipitate was collected by filtration. The collected solid was recrystallized from hexane to afford 1.8 g of N-[3-cyano-4-(1,1-dimethylethyl)-2-thienyl]-3-methyl-2-pyrrolidinone. Yield 75%. mp=92°-94° C.

Aufarbeitung

  1. customthe solvent was removed in vacuo
  2. filtrationthe precipitate was collected by filtration
  3. customThe collected solid was recrystallized from hexane

Quellen und Nachweise

ORD-Eintrag
ord-df30eafc0ee543eb824b4181757cfbd0
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04643758

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