Реакция #985298

ord-7c669845a24a43bb8a9dda151da4a71a

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooled in ice
  2. 2
    Температураwithout cooling
  3. 3
    ЭкстракцияExtraction
  4. 4
    workup.DISTILLATIONDistillation
  5. 5
    Другое75° C./20 mbar

Методика

N,O-dimethyl-hydroxylamine HCl (40 g, 410 mmol) was suspended under nitrogen in DCM (400 mL) and cooled in ice. Triethylamine (63 mL, 451 mmol) was added slowly, then cyclopropanecarbonyl chloride (41 mL, 451 mmol) was added slowly. Stirring without cooling was continued for 1 h. Extraction: 2×DCM, 1×1 N HCl, 1×NaCl. Distillation: 75° C./20 mbar. One obtained 32.5 g (61%) of a colorless oil.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07351700B2uspto-grants-2008_04