反応 #67962

ord-1a20acba42b44c2fb88c7da546c2a2e8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the solvent was removed under reduced pressure
  2. 2
    その他The residue thus obtained
  3. 3
    その他The aqueous layer was separated
  4. 4
    workup.ADDITIONethyl acetate was added
  5. 5
    その他The organic layer was separated
  6. 6
    乾燥dried over potassium carbonate
  7. 7
    その他the solvent was removed under reduced pressure

実験手順

To 0.60 g of 1-tert-butyl 3-ethyl 4-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-1,3-dicarboxylate, 12 mL of 10 mol/L hydrogen chloride/ethanol was added, and the mixture was stirred for 2 hours, and then the solvent was removed under reduced pressure. The residue thus obtained was added with water and ethyl acetate. The aqueous layer was separated, ethyl acetate was added thereto, and the resultant solution was adjusted to pH 14 with a 5 mol/L aqueous sodium hydroxide solution. The organic layer was separated and dried over potassium carbonate, and the solvent was removed under reduced pressure to obtain 0.34 g of a brown oily substance, ethyl 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-2-carboxylate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08524738B2uspto-grants-2013_09