反応 #59636

ord-2870f34e8b1c47c59fdc29725e9d888c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他This compound is prepared
  2. 2
    温度the mixture is then refluxed for 30 minutes
  3. 3
    抽出it is extracted with EtOAc
  4. 4
    乾燥the organic phase is dried over Na2SO4
  5. 5
    その他the solvent is evaporated off under vacuum
  6. 6
    その他the precipitate formed
  7. 7
    ろ過is spin-filtered off

実験手順

This compound is prepared according to the process described in Organic Syntheses, 1925, V, 71-74. A solution of 16.5 ml of concentrated HCl in 120 ml of water and a solution of 41.5 g of hydroxylamine hydrochloride in 70 ml of water are added to a mixture of 25 g of 5-aminoindane, 35 g of chloral hydrate and 22 g of Na2SO4 in 600 ml of water, and the mixture is then refluxed for 30 minutes. After cooling the reaction mixture to RT, it is extracted with EtOAc, the organic phase is dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is taken up in a pentane/iso ether mixture and the precipitate formed is spin-filtered off. 23 g of the expected product are obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07425566B2uspto-grants-2008_09