반응 #47945

ord-6ed28fddb3784930a872ce9efc7b88b1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the mixture was extracted with ethyl acetate
  2. 2
    세척The organic phase was washed with brine
  3. 3
    건조dried over anhydrous Na2SO4
  4. 4
    여과filtered
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The crude product was purified by a silica SPE cartridge (10 g)
  7. 7
    세척eluting with dichloromethane/methanol from 100/0 to 99/1

실험 절차

To a solution of 2-(methylthio)-4-[(phenylmethyl)oxy]pyrimidine (P9, 245 mg) in THF/MeOH 1/1 (15.6 mL) was added a solution of Oxone® (2.6 g) in water (14 mL). After 40 min a saturated NaHCO3 solution was added and the mixture was extracted with ethyl acetate. The organic phase was washed with brine, dried over anhydrous Na2SO4 filtered and concentrated under reduced pressure. The crude product was purified by a silica SPE cartridge (10 g) eluting with dichloromethane/methanol from 100/0 to 99/1 to give the title compound as a white solid (230 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745458B2uspto-grants-2010_06