Reaktion #1333374

Reaktionsgleichung

HCl

HCl

intermediate ( 9 )

1-acetyl-5-chloro-2,3-dihydro-1H-indole-2-carbonitrile

ethanol

HCl

HCl

→

ethyl 1-acetyl-5-chloro-2,3-dihydro-1H-indole-2-carboximidate monohydrochloride

Lösungsmittel

diethylether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprecipitating out
2. 2
   workup.ADDITIONThe reaction was diluted to 1 l with diethylether
3. 3
   SonstigeMore oil precipitates
4. 4
   Sonstigeno solid formed
5. 5
   SonstigeThe diethylether was decanted off
6. 6
   workup.ADDITIONThe residue was diluted (diethylether, 500 ml)
7. 7
   Sonstigeto form
8. 8
   FiltrationThe sample was filtered
9. 9
   Waschenrinsing with diethylether

Vorschrift

HCl (as a 2 M solution) was added slowly to intermediate (9) until gas evolution was noted. Then stopped adding the prepared HCl (2N in diethylether), and suspended HCl in diethylether (150 ml) and then ethanol (0.042 mole) was added. The mixture was cooled to 0° C. and HCl (gas) was added over an hour, with an oil precipitating out. The reaction was diluted to 1 l with diethylether. More oil precipitates, and no solid formed after sitting for 1 hour. The diethylether was decanted off. The residue was diluted (diethylether, 500 ml). The solid begins to form, and the mixture was stirred for 2 hours. The sample was filtered, rinsing with diethylether. The sample was placed under vacuum, yielding 6.41 g of ethyl 1-acetyl-5-chloro-2,3-dihydro-1H-indole-2-carboximidate monohydrochloride (intermediate 10).

Quelle