Reaktion #798676

ord-4494c80ef4ba42c3acd938f5a46c11f5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONThe reaction mixture was poured slowly onto ice
  2. 2
    Sonstigeto yield a pale yellow precipitate
  3. 3
    Sonstigewhich was isolated by vacuum filtration
  4. 4
    Waschenwashed with water
  5. 5
    Sonstigedried under vacuum

Vorschrift

A solution of ethyl 4-(1,5-dimethyl-1H-pyrazol-4-yl)-6-methyl-2-(methylsulfonyl)pyrimidine-5-carboxylate (0.07 g, 0.207 mmol), tert-butyl (1S,2R)-2-aminocyclohexylcarbamate (0.089 g, 0.414 mmol) and Et3N (0.115 mL, 0.827 mmol) in DMA (3 mL) was heated in a sealed tube at 90° C. for 8 h. The reaction mixture was poured slowly onto ice to yield a pale yellow precipitate, which was isolated by vacuum filtration, washed with water, and dried under vacuum to give the title compound. [M+H] calc'd for C24H36N6O4, 473. found, 473.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09181255B2uspto-grants-2015_11