반응 #70120

ord-1158d82d9aa24d7db4dbdc5a06a5f6fd

용매

반응 조건

온도
-16°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was fed to the solution at a temperature below 20° C
  2. 2
    기타Nitrogen gas was bubbled
  3. 3
    농축The reaction solution was concentrated
  4. 4
    기타was separated

실험 절차

In 50 g of methanol were dissolved 10 g (0.069 mol) of 1-naphthol and 7.2 g (0.069 mol) of tetramethylene sulfoxide. The solution was cooled to −16° C. An excess of hydrogen chloride gas was fed to the solution at a temperature below 20° C. Nitrogen gas was bubbled to expel the excess of hydrogen chloride. The reaction solution was concentrated and combined with water and diisopropyl ether, from which a water layer was separated. It was an aqueous solution of 4-hydroxynaphthyl-1-tetrahydrothiophenium chloride. This aqueous solution was used in the subsequent step without further isolation.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08535869B2uspto-grants-2013_09