Reaktion #70339

ord-5f9f7668ae5242c081121df1294b9a7b

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe solvent was evaporated
  2. 2
    Sonstigethe solid obtained
  3. 3
    Extraktionextracted with CHCl3
  4. 4
    SonstigeThe crude mixture was purified over a SiO2 eluting with DCM/MeOH 2%

Vorschrift

The solid residue obtained in step A was dissolved in methanol (3 ml) and aqueous solution 2N NaOH (1 ml) was added. The mixture was heated at 60° C. for 2 hours, the solvent was evaporated and the solid obtained was suspended in water. The pH was taken to 6.5 and extracted with CHCl3. The crude mixture was purified over a SiO2 eluting with DCM/MeOH 2% affording 0.170 g (yield 81%) of the expected product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536165B2uspto-grants-2013_09