반응 #59636

ord-2870f34e8b1c47c59fdc29725e9d888c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타This compound is prepared
  2. 2
    온도the mixture is then refluxed for 30 minutes
  3. 3
    추출it is extracted with EtOAc
  4. 4
    건조the organic phase is dried over Na2SO4
  5. 5
    기타the solvent is evaporated off under vacuum
  6. 6
    기타the precipitate formed
  7. 7
    여과is spin-filtered off

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425566B2uspto-grants-2008_09