反応 #4742

ord-19bba1e04b7a4a7cafd3ccb58c5285a5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度When cooled
  2. 2
    温度with cooling
  3. 3
    抽出The product is extracted with ether
  4. 4
    洗浄the combined ether extracts are washed
  5. 5
    濃縮concentrated by evaporation
  6. 6
    その他The solid residue is recrystallised from ether

実験手順

7 mmol of N-[2-Methyl-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-1,2-hydrazine dicarboxamide in 30 ml of phosphorus oxychloride are stirred for 6 hours at 50°-60° C. When cooled, the reaction mixture is poured out on 300 ml of ice water and neutralized by the addition of concentrated ammonia solution with cooling. The product is extracted with ether and the combined ether extracts are washed, dehydrated and concentrated by evaporation. The solid residue is recrystallised from ether.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727081uspto-grants-1988_02