Reaktion #91198

ord-c337f1ec19ba43a3a3c333ed971ca393

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter the termination of the reaction
  2. 2
    Einengenthe reactant was concentrated under reduced pressure
  3. 3
    workup.ADDITIONthe residue was diluted with water
  4. 4
    workup.ADDITIONThe aqueous layer was added with diethyl ether
  5. 5
    workup.STIRRINGstirred
  6. 6
    Extraktionextracted
  7. 7
    workup.ADDITIONThe aqueous layer was added with 1N HCl
  8. 8
    Extraktionextracted with EtOAc
  9. 9
    TrocknenThe organic layer was dried with MgSO4
  10. 10
    Einengenconcentrated under reduced pressure

Vorschrift

After 3-[3,5-difluoro-4-(2-isopropylsulfanyl-pyridin-3-ylmethoxy)phenyl]-propionic acid ethyl ester (66 mg, 0.167 mmol) obtained in Step A was dissolved in THF/MeOH/water (2:2:1, 5 mL), lithium hydroxide (12 mg, 0.50 mmol) was added thereto, and the mixture was stirred at room temperature for 2 hours. After the termination of the reaction, the reactant was concentrated under reduced pressure, and the residue was diluted with water. The aqueous layer was added with diethyl ether, stirred, and then extracted. The aqueous layer was added with 1N HCl to adjust pH to 2˜3, and then extracted with EtOAc. The organic layer was dried with MgSO4, and concentrated under reduced pressure to obtain the title compound (56 mg, 91%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447044B2uspto-grants-2016_09