Реакция #70120

ord-1158d82d9aa24d7db4dbdc5a06a5f6fd

Реагенты

Нет

Растворители

Условия реакции

Температура
-16°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеwas fed to the solution at a temperature below 20° C
  2. 2
    ДругоеNitrogen gas was bubbled
  3. 3
    КонцентрированиеThe reaction solution was concentrated
  4. 4
    Другоеwas separated

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08535869B2uspto-grants-2013_09