Реакция #67947

ord-93e876b0154a43d2a9ecd0e7b7dab8bb

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwere added at 5° C.
  2. 2
    ДругоеThe organic layer was separated
  3. 3
    Экстракцияthe aqueous layer was extracted with ethyl acetate
  4. 4
    Промывкаthe resultant solution was washed with an aqueous saturated sodium chloride solution
  5. 5
    Сушкаdried over anhydrous magnesium sulfate
  6. 6
    Другоеthe solvent was removed under reduced pressure

Методика

To 20 mL of a tetrahydrofuran solution containing 1.7 g of 1-tert-butyl 4-ethyl 4-(3-hydroxypropyl)piperidine-1,4-dicarboxylate, 0.82 mL of triethylamine and 0.58 mL of methane sulfonylchloride were added at 5° C., and the mixture was stirred at room temperature for 1 hour. Ethyl acetate and water were added thereto. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 1.9 g of a colorless oily substance, 1-tert-butyl 4-ethyl 4-(3-((methanesulfonyl)oxy)propyl)piperidine-1,4-dicarboxylate.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08524738B2uspto-grants-2013_09