Reaktion #10495

ord-98cc223bf38a4ce9a090aa143a53649e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONadded to the above solution
  2. 2
    SonstigeAfter the completion the mixture was quenched with water
  3. 3
    Extraktionextracted with CH2Cl2
  4. 4
    ExtraktionThe aqueous layer was extracted again with more CH2Cl2
  5. 5
    TrocknenThe combined methylene chloride layer was dried over anhydrous MgSO4
  6. 6
    Filtrationfiltered
  7. 7
    SonstigeRemoval of solvent
  8. 8
    Sonstigegave crude product with a yield of 1.11 g

Vorschrift

(5-Bromo-benzothiazol-2-yl)-acetic acid ethyl ester (1.25 g, 4.2 mmol) was dissolved in THF (20 mL) and EtOH (5 mL) under N2. Then 0.24 g of NaBH4 was dissolved in EtOH (3 mL) and added to the above solution. The reaction mixture was stirred at room temperature for 2 hours. After the completion the mixture was quenched with water and extracted with CH2Cl2. The aqueous layer was extracted again with more CH2Cl2. The combined methylene chloride layer was dried over anhydrous MgSO4 and filtered. Removal of solvent gave crude product with a yield of 1.11 g. The crude product was used directly in the next step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07094790B2uspto-grants-2006_08