Реакция #64960

ord-f28620367f2047f1853653cedc0a5f76

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe BaCO3 is filtered off with suction, K2CO3
  2. 2
    workup.ADDITIONis added to the filtrate
  3. 3
    Фильтрацияthe solid is filtered off with suction again
  4. 4
    Экстракцияthe filtrate is extracted ten times with 100 ml of CHCl3 each time
  5. 5
    СушкаThe extracts are dried over K2CO3
  6. 6
    Концентрированиеconcentrated
  7. 7
    workup.DISTILLATIONthe residue is distilled

Методика

13 g (60.6 mmol) of ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 33 g of Ba(OH)2.8H2O in 330 ml of water overnight. The BaCO3 is filtered off with suction, K2CO3 is added to the filtrate, the solid is filtered off with suction again and the filtrate is extracted ten times with 100 ml of CHCl3 each time. The extracts are dried over K2CO3 and concentrated and the residue is distilled.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05416096uspto-grants-1995_05