Reaktion #2061938

ord-f8dc75b1958c49ffb6f6233a266fab05

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwith cooling in an ice bath
  2. 2
    SonstigeThe reaction mixture is quenched sequentially with 0.8 ml of water, 0.8 ml of 15% NaOH aqueous solution, and 2.4 ml of water
  3. 3
    FiltrationThe resulting white precipitate is filtered off
  4. 4
    Waschenwashed thoroughly with diethyl ether
  5. 5
    Einengenconcentrated

Vorschrift

LiAlH4 (0.77 g, 20.4 mmol) is suspended in 30 ml of dry diethyl ether with cooling in an ice bath. 2-(4--fluorophenylthio)-6-fluorobenzoic acid (4.53 g, 17.0 mmol) in 6 ml of diethyl ether and 6 ml of THF is then added and the reaction mixture stirred at room temperature overnight. The reaction mixture is quenched sequentially with 0.8 ml of water, 0.8 ml of 15% NaOH aqueous solution, and 2.4 ml of water. The resulting white precipitate is filtered off and washed thoroughly with diethyl ether. The filtrate and washings are combined and concentrated to afford the subtitle compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05283361uspto-grants-1994_02