反応 #3242

ord-8547a040ad9a425c98f22d4b4c6c403c

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent was evaporated
  2. 2
    濃縮the reaction solution was concentrated
  3. 3
    workup.ADDITIONmethylene chloride was added
  4. 4
    ろ過followed by filtration
  5. 5
    濃縮The filtrate was concentrated
  6. 6
    その他the resulting oily substance was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)

実験手順

To a solution of 9.6 g of 2-isopropylaminobenzyl alcohol in 200 ml of dioxane was added 13.2 g of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) in several portions, followed by stirring for an hour. The solvent was evaporated, the reaction solution was concentrated, and methylene chloride was added thereto, followed by filtration. The filtrate was concentrated, and the resulting oily substance was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to give 7.6 g of 2-isopropylaminobenzaldehyde.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05733917uspto-grants-1998_03