Reaction #1265406

ord-d909c6680d2e4f75b512f0eda1e5f87d

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturewas refluxed for 1 hour until a clear solution
  2. 2
    Otherwas formed
  3. 3
    TemperatureBy cooling down the reaction mixture in the refrigerator
  4. 4
    Otherthe precipitate formed
  5. 5
    Filtrationwas filtered off
  6. 6
    Washwashed with ethyl acetate and diethyl ether
  7. 7
    Dryingdried over P2O5 under vacuum

Procedure

A suspension of the compound of example 101 (10.46 g, 35 mmoles) in acetic anhydride (600 ml) and acetic acid (200 ml) was refluxed for 1 hour until a clear solution was formed. By cooling down the reaction mixture in the refrigerator, the precipitate formed was filtered off, washed with ethyl acetate and diethyl ether, and then dried over P2O5 under vacuum, providing the title compound as a yellow powder (9.19 g, yield: 77%). This compound was further characterized by the following spectra:

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07276506B2uspto-grants-2007_10