反応 #70120

ord-1158d82d9aa24d7db4dbdc5a06a5f6fd

反応方程式

Oc1cccc2ccccc12
1-naphthol
O=S1CCCC1
tetramethylene sulfoxide
Cl
hydrogen chloride
Oc1ccc([S+]2CCCC2)c2ccccc12.[Cl-]
4-hydroxynaphthyl-1-tetrahydrothiophenium chloride

溶媒

反応条件

温度
-16°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was fed to the solution at a temperature below 20° C
  2. 2
    その他Nitrogen gas was bubbled
  3. 3
    濃縮The reaction solution was concentrated
  4. 4
    その他was separated

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08535869B2uspto-grants-2013_09