Reaktion #217120

ord-0ddd88e06c914d409db09cfbfbdd4f84

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is heated
  2. 2
    Temperaturto reflux for 1 h
  3. 3
    Filtrationis filtered off from the precipitate with suction
  4. 4
    TrocknenThe combined mother liquors are dried over magnesium sulphate
  5. 5
    Einengenconcentrated in vacuo
  6. 6
    Filtrationfiltered off with suction
  7. 7
    Sonstigedried in a desiccator

Vorschrift

20.7 g (57.7 mmol) of the compound from Example 26 dissolved in 50 ml of absolute tetrahydrofuran are slowly added dropwise under nitrogen to a suspension of 6 g (158 mmol) of lithium aluminum hydride in 200 ml of absolute tetrahydrofuran at 60° C. The mixture is heated to reflux for 1 h, cooled to 0° C. and 18 ml of water are cautiously added. 6 ml of 10% strength potassium hydroxide solution are added to the mixture, it is filtered off from the precipitate with suction and the residue is boiled twice using 250 ml of ether each time. The combined mother liquors are dried over magnesium sulphate and concentrated in vacuo. The residue is stirred with petroleum ether, filtered off with suction and dried in a desiccator.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05470982uspto-grants-1995_11