Reacción #59636

Ecuación de reacción

HCl

hydroxylamine hydrochloride

5-aminoindane

chloral hydrate

Na2SO4

→

expected product

Rendimiento 60.0%

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

Rendimiento 60.0%

Disolventes

water

water

water

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThis compound is prepared
2. 2
   Temperaturathe mixture is then refluxed for 30 minutes
3. 3
   Extracciónit is extracted with EtOAc
4. 4
   Secadothe organic phase is dried over Na2SO4
5. 5
   Otrothe solvent is evaporated off under vacuum
6. 6
   Otrothe precipitate formed
7. 7
   Filtraciónis spin-filtered off

Procedimiento

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.

Fuente