Реакция #985244

ord-943b16cb7d5b46f6a0f07b568d191b7f

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added dropwise at 10-25° C.
  2. 2
    Другоеfollowed by reaction at room temperature for 2.5 hours
  3. 3
    КонцентрированиеThe reaction solution was concentrated at room temperature under reduced pressure
  4. 4
    ПромывкаThe resulting oily residue was washed with H2O several times
  5. 5
    Сушкаdried over anhydrous MgSO4
  6. 6
    ДругоеAfter removing the drying agent
  7. 7
    Фильтрацияby filtration

Методика

After dissolving sodium azide (22.5 g, 0.35 mole) in a small amount of H2O, the resulting solution was diluted with a 90% ethanol aqueous solution (130 ml). To this, an ethanol solution dissolving p-toluenesulfonyl chloride (60 g, 0.32 mole) was added dropwise at 10-25° C., followed by reaction at room temperature for 2.5 hours. The reaction solution was concentrated at room temperature under reduced pressure. The resulting oily residue was washed with H2O several times and dried over anhydrous MgSO4. After removing the drying agent by filtration, there was obtained 50.7 g of the title compound as a colorless oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE040211E1uspto-grants-2008_04