Реакция #977212

ord-0961fd66930f4fb799f84d3e9b59c80c

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwere added
  2. 2
    ФильтрацияThe reaction mixture was filtered
  3. 3
    Концентрированиеthe filtrate was concentrated under reduced pressure
  4. 4
    workup.ADDITIONAfter adding water
  5. 5
    Экстракцияto the residue, extraction
  6. 6
    ПромывкаThe organic layer was washed with water
  7. 7
    Сушкаdried over anhydrous magnesium sulfate
  8. 8
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Методика

After dissolving 106 mg of 7-(tert-butoxycarbonyl)-2-hydroxy-7-azaspiro[3.5]nonane in 10 ml of tetrahydrofuran, 0.04 ml of methanesulfonyl chloride and 0.07 ml of triethylamine were added and the mixture was stirred overnight at room temperature. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. After adding water to the residue, extraction was performed with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (148 mg, 100% yield).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06995144B2uspto-grants-2006_02