Reaction #1810826

ord-a3604cbf8d3f4f38aca16fb7d4486071

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturewas heated for 16 h to 100° C
  2. 2
    OtherAfter evaporation of all volatiles the residue
  3. 3
    Othersubjected to reversed phase HPLC purification
  4. 4
    Washeluting with an acetonitrile/water gradient
  5. 5
    Otherto yield
  6. 6
    Otherafter evaporation of the product fractions the title compound

Procedure

A mixture of 163.8 mg (0.7 mmol) 2-chloro-5-methanesulfonyl-benzoic acid (example 4 step b) in 2 ml morpholine was heated for 16 h to 100° C. After evaporation of all volatiles the residue was taken up in 2 ml methanol/formic acid 3/1 and subjected to reversed phase HPLC purification eluting with an acetonitrile/water gradient to yield after evaporation of the product fractions the title compound. MS (m/e): 284.1 (M−H, 100%)

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07485637B2uspto-grants-2009_02