반응 #895

ord-bbaa547034cb4578bce2648d1c091a1f

반응 방정식

C[S-].[Na+]
sodium thiomethoxide
Clc1cc(Cl)nc(OCc2ccccc2)n1
4,6-dichloro-2-(phenylmethoxy)pyrimidine
CSc1cc(Cl)nc(OCc2ccccc2)n1
4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to react for 2 hours
  2. 2
    기타the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
  3. 3
    세척The organic layer was washed with aqueous saturated sodium chloride
  4. 4
    건조dried over anhydrous sodium sulfate
  5. 5
    농축concentrated
  6. 6
    기타purified on a silica gel column

실험 절차

Aqueous sodium thiomethoxide (15%, 2.75 g, 0.0059×1.0 mol) was added dropwise in 4,6-dichloro-2-(phenylmethoxy)pyrimidine (Compound No. II-26) (1.5 g, 0.0059 mol) dissolved in THF at room temperature. After allowed to react for 2 hours, the reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, then purified on a silica gel column to obtain 4-chloro-6-methylthio-2-(phenylmethoxy)pyrimidine (Compound No. II-15) as an intermediate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723412uspto-grants-1998_03