Reacción #64964

ord-382fd6d71893401b82ac7f63aa2dec0a

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe BaCO3 is filtered off with suction, K2CO3
  2. 2
    workup.ADDITIONis added to the filtrate
  3. 3
    Filtraciónthe solid is filtered off with suction again
  4. 4
    ExtracciónThe filtrate is extracted ten times with 50 ml of CHCl3 each time
  5. 5
    Secadothe extracts are dried over K2CO3
  6. 6
    Concentraciónconcentrated
  7. 7
    workup.DISTILLATIONthe residue is distilled

Procedimiento

9.2 g (42.9 mmol) of ethyl 2,8-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 23.5 g of Ba(OH)2.8H2O in 235 ml of water overnight. The BaCO3 is filtered off with suction, K2CO3 is added to the filtrate and the solid is filtered off with suction again. The filtrate is extracted ten times with 50 ml of CHCl3 each time, the extracts are dried over K2CO3 and concentrated and the residue is distilled.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05416096uspto-grants-1995_05