反応 #53437

ord-8e64fb0de175486682f4ed35ca9f9ed1

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    乾燥The resulting suspension is dried (Na2SO4)
  2. 2
    ろ過filtered through celite
  3. 3
    濃縮After concentration under reduced pressure
  4. 4
    その他the white solid (34.0 g) is crystallized from EtOAc/hexanes

実験手順

To a suspension of lithium aluminum hydride (10.6 g, 264 mmol) in THF (200 mL) is added dropwise a solution of ethyl indole-2-carboxylate (50.0 g, 256 mmol) in THF (250 mL) over 25 minutes. After 3 h, water (10.6 mL) is carefully added, followed by 15% NaOH (10.6 mL), followed by additional portion of water (31.8 mL). The resulting suspension is dried (Na2SO4) and filtered through celite. After concentration under reduced pressure, the white solid (34.0 g) is crystallized from EtOAc/hexanes to give white needles for 1H-indol-2-ylmethanol. Yield 83%. HRMS (FAB) calcd for C9H9NO+H 148.0762, found 148.0771.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06858613B2uspto-grants-2005_02