반응 #64981

ord-352dfc76302b4aa0b96f5e64bf68c735

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux
  2. 2
    여과The salts are filtered off
  3. 3
    농축the filtrate is concentrated by evaporation
  4. 4
    workup.DISTILLATIONthe residue is distilled

실험 절차

13.0 g of crude 5-methyl-hexahydropyridine-2,3-dicarboxylic acid N-benzylimide are added in the form of a solution in 50 ml of absolute tetrahydrofuran to 4.6 g (0.12 mol) of lithium aluminum hydride in 100 ml of absolute tetrahydrofuran, already present in the vessel. Then the mixture is boiled for 17 hours under reflux. 4.6 g of water in 14 ml of tetrahydrofuran, 4.6 g of 10% strength sodium hydroxide solution and 13.8 g of water are added dropwise one after the other. The salts are filtered off, the filtrate is concentrated by evaporation and the residue is distilled.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05416096uspto-grants-1995_05