Реакция #40915

ord-68c8ac8859e74626b8a337ceb841d865

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted
  2. 2
    workup.ADDITIONafter adding water (80 ml)
  3. 3
    СушкаThe organic phase was dried over sodium sulfate
  4. 4
    Концентрированиеconcentrated by evaporation in vacuo
  5. 5
    Другоеthe product was obtained as a white solid

Методика

40% aqueous dimethylamine solution (85 ml, 0.67 mole), 1,4-dioxa-spiro-[4.5]decane-8-carbaldehyde 5 (240 g, 0.141 mole) and potassium cyanide (22.05 g, 0.338 mole) were added while cooling with ice to a mixture of 4N hydrochloric acid (37 ml) and methanol (22 ml). The mixture was stirred for four days at room temperature and then extracted, after adding water (80 ml), with diethyl ether (4×100 ml). The organic phase was dried over sodium sulfate, concentrated by evaporation in vacuo, and the product was obtained as a white solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07728028B2uspto-grants-2010_06