Reaction #155732

ord-480b9947a2fb41b6ab3655deb9dd0a1b

Solvents

Conditions

Temperature
60°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    TemperatureThe reaction was cooled
  2. 2
    Filtrationthe precipitate was filtered
  3. 3
    OtherThe filtrate was evaporated
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in DCM
  5. 5
    Extractionextracted with water
  6. 6
    Washwashed with sodium chloride solution
  7. 7
    OtherThe solvent was evaporated
  8. 8
    Otherthe residue was crystallized with a mixture of petrolether and diethylether (8:2)

Procedure

18.6 mL triethylamine and piperazine-1-carboxylic acid tert-butyl ester were added to 9.7 g 4-chloro-6-methoxy-pyrimidine in 50 mL DMF. The reaction was stirred over night at 60° C. The reaction was cooled and the precipitate was filtered. The filtrate was evaporated. The residue was dissolved in DCM, extracted with water and washed with sodium chloride solution. The solvent was evaporated and the residue was crystallized with a mixture of petrolether and diethylether (8:2) to yield 8.7 g of the desired compound.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822464B2uspto-grants-2014_09