Reaktion #59636

Reaktionsgleichung

HCl

hydroxylamine hydrochloride

5-aminoindane

chloral hydrate

Na2SO4

→

expected product

Ausbeute 60.0%

N-(2,3-Dihydro-1H-inden-5-yl)-2-(hydroxyimino)acetamide

Ausbeute 60.0%

Lösungsmittel

water

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThis compound is prepared
2. 2
   Temperaturthe mixture is then refluxed for 30 minutes
3. 3
   Extraktionit is extracted with EtOAc
4. 4
   Trocknenthe organic phase is dried over Na2SO4
5. 5
   Sonstigethe solvent is evaporated off under vacuum
6. 6
   Sonstigethe precipitate formed
7. 7
   Filtrationis spin-filtered off

Vorschrift

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.

Quelle