تفاعل #59636

ord-2870f34e8b1c47c59fdc29725e9d888c

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThis compound is prepared
  2. 2
    درجة الحرارةthe mixture is then refluxed for 30 minutes
  3. 3
    استخلاصit is extracted with EtOAc
  4. 4
    تجفيفthe organic phase is dried over Na2SO4
  5. 5
    أخرىthe solvent is evaporated off under vacuum
  6. 6
    أخرىthe precipitate formed
  7. 7
    ترشيحis spin-filtered off

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425566B2uspto-grants-2008_09