Реакция #40919

ord-85f0a1c8da154ceeb53790dd29fb205d

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted with diethyl ether (4×100 ml)
  2. 2
    СушкаThe organic phase was dried over sodium sulfate
  3. 3
    Концентрированиеconcentrated by evaporation in vacuo
  4. 4
    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, after adding water (80 ml), extracted 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