Reaction #53429

ord-a00cbcb54b8f47ee845db3020a23743c

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    OtherThe reaction mixture is evaporated in vacuo
  2. 2
    Otherthe mixture is evaporated again
  3. 3
    Extractionextracted several times with water
  4. 4
    OtherThe aqueous phase is evaporated to a very great extent
  5. 5
    Otheran oil being obtained which
  6. 6
    Othercrystallizes on standing

Procedure

3.0 g (16.4 mmol) of the compound from Example I are boiled under reflux for 17 hours in 250 ml of a saturated methanolic ammonia solution. The reaction mixture is evaporated in vacuo, the residue is taken up in methanol and the mixture is evaporated again; this process is repeated a few times. The crude product is taken up in dichloromethane and extracted several times with water. The aqueous phase is evaporated to a very great extent, an oil being obtained which crystallizes on standing.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858622B2uspto-grants-2005_02