Reaktion #1472213

ord-9fdd006d23c84e68816f4a08d800cf40

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    WaschenThe alkaline phase was washed with ethyl acetate and diethyl ether
  2. 2
    FiltrationThe precipitate was filtered off under suction
  3. 3
    Extraktionthe aqueous phase was extracted with ethyl acetate
  4. 4
    SonstigeThis organic phase was dried
  5. 5
    Einengenconcentrated

Vorschrift

1.00 g of 8-bromoquinoline-5-carboxylic acid, 0.44 g of 1-ethyl-5-hydroxypyrazole and 0.80 g of dicyclohexylcarbodiimide were stirred in 15 ml of acetonitrile at room temperature. After the addition of 0.2 ml of acetone cyanohydrin and 0.60 g of triethylamine, stirring was continued for 1.5 hours and the mixture was then poured into aqueous sodium carbonate solution. The alkaline phase was washed with ethyl acetate and diethyl ether and then acidified. The precipitate was filtered off under suction and the aqueous phase was extracted with ethyl acetate. This organic phase was dried and concentrated. The residue and the precipitate were combined.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06262074B1uspto-grants-2001_07