반응 #6793

ord-7489cadc00124f82a4089f651da7299f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe mixture stirred overnight
  2. 2
    농축The reaction mixture was concentrated in vacuo
  3. 3
    기타the residue partitioned between dichloromethane (20 ml) and water (20 ml)
  4. 4
    기타The organic layer was purified
  5. 5
    세척elute column
  6. 6
    세척eluting with dichloromethane

실험 절차

A solution of 4-[4-(methylsulfonyl)phenyl]-N-tetrahydro-2H-pyran-4-yl-6-(trifluoromethyl)pyrimidin-2-amine (0.05 g) in dry dimethylformamide (2 ml) was treated with sodium hydride (0.007 g, 60% in mineral oil) and the mixture stirred at ambient temperature for 30 minutes. Iodomethane (0.01 ml) was added and the mixture stirred overnight. The reaction mixture was concentrated in vacuo and the residue partitioned between dichloromethane (20 ml) and water (20 ml). The organic layer was purified by passing through a silica bond elute column and eluting with dichloromethane. Concentration of the eluent gave the title compound as a yellow solid (0.031 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084148B2uspto-grants-2006_08