反応 #72918

ord-e7e685d6fe9e494f97c7dc5fcc2eda18

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the suspension was cooled
  2. 2
    ろ過filtered
  3. 3
    workup.ADDITIONpH was adjusted to 10 through portionwise addition of Na2CO3 to the aqueous phase
  4. 4
    抽出Extraction with dichloromethane

実験手順

To a solution of 840 mg (3.189 mmol) of 1-tert-butyl-4-(4-nitrophenyl)piperazine in 24 mL of methanol, 904 mg (16.9 mmol) of ammonium chloride dissolved in 6 mL of water and 552 mg (9.886 mmol) of iron were added. After 7 hours, the suspension was cooled and filtered. pH was adjusted to 10 through portionwise addition of Na2CO3 to the aqueous phase. Extraction with dichloromethane yielded 667 mg of the title amine.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541429B2uspto-grants-2013_09