Reaction #155490

ord-eb710248ab6c4f938a4f3cbc762656e6

Solvents

Conditions

Temperature
25°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    OtherThe solvents were evaporated under reduced pressure
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in water
  3. 3
    Extractionextracted with ethyl acetate
  4. 4
    ExtractionThe combined ethyl acetate extract
  5. 5
    Washwas washed with water & brine
  6. 6
    Dryingdried over sodium sulphate

Procedure

To a solution of the product of step 3 (28 g, 0.0683 moles) in THF (140 ml), a solution of lithium hydroxide (4.3 g, 0.1024 moles) in water (140 ml) was added and the reaction mixture was stirred at 25° C. for 3 hours. The solvents were evaporated under reduced pressure. The residue was dissolved in water, acidified with 1N HCl and extracted with ethyl acetate. The combined ethyl acetate extract was washed with water & brine, dried over sodium sulphate and evapourated under reduced pressure to yield 23 gm (88%) of product as solid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822414B2uspto-grants-2014_09