Reaktion #936227

Reaktionsgleichung

title product

4,5,6,7-tetrahydro-2-methoxy-7-(phenylmethyl)-2H-azepine

ammonium chloride

→

white solid

Ausbeute 92.0%

hexahydro-7-(phenylmethyl)-2H-azepin-2-imine, monohydrochloride

Ausbeute 92.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   Sonstigethe reaction to room temperature
3. 3
   Filtrationit was filtered
4. 4
   Sonstigepartitioned between 15 mL of water and 7 mL of CH2Cl2
5. 5
   SonstigeThe organic and aqueous phases were separated
6. 6
   Waschenthe aqueous phase was washed with a 25 mL portion of EtOAc before it

Vorschrift

The title product of Example 3 (0.30 g, 1.4 mmol) and 0.06 g (1.1 mmol) of ammonium chloride (NH4Cl) were refluxed in 13 mL of methanol (MeOH) under a nitrogen atmosphere for 19 h. After cooling the reaction to room temperature, it was filtered, stripped of all solvent under reduced pressure, and partitioned between 15 mL of water and 7 mL of CH2Cl2. The organic and aqueous phases were separated and the aqueous phase was washed with a 25 mL portion of EtOAc before it was lyophilized to provide 0.24 g (92%) of the white solid title material.

Quelle