Reaktion #684350

Reaktionsgleichung

HCl

1-amino-1,2,3,5-tetrahydro4,1-benzoxazepine hydrochloride

1,2,8,9,10,11-hexahydro-4H-pyrido[3',4':4,5]pyrrolo[3,2,1-jk][4,1]benzoxazepine

→

1,2,8,9,10,11-hexahydro-4H-pyrido[3',4':4,5]pyrrolo[3,2,1-jk][4,1]benzoxazepine hydrochloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationis filtered
2. 2
   Waschenwashed on the
3. 3
   Filtrationfilter with ether, m.p. 229°-230°
4. 4
   SonstigeThe aforementioned hydrazine hydrochloride (3 g.) is reacted with 2.6 g of 4-piperidone hydrochloride in 30 ml of ethanol saturated with gaseous HCl
5. 5
   Temperaturby heating
6. 6
   Temperaturto reflux for 2 hours
7. 7
   TemperaturThe product was cooled
8. 8
   Filtrationfiltered
9. 9
   Sonstigerecrystallized from ethanol
10. 10
    Sonstigewas 296°-297°

Vorschrift

1,2,3,5-Tetrahydro-4,1-benzoxazepine, prepared according to E. Testa and L. Fontanella, Fr. Pat. No. 1,405,271, is converted to the corresponding 5-nitroso derivative as described in Example 1 obtained as yellow crystals, m.p. 62°-64° C. The latter, 8.3 g, is dissolved in 130 ml of methanol. To the resulting solution, cooled to 10°-15° C. there is added 20 g of Zn dust in small portions along with 25 ml of acetic acid, added dropwise. After the addition is complete, the mixture is stirred at room temperature for 3 hours and then filtered. The filtrate is stripped of the solvent under reduced pressure and the oily residue is treated with 5N HCl to yield 1-amino-1,2,3,5-tetrahydro4,1-benzoxazepine hydrochloride, which is filtered and washed on the filter with ether, m.p. 229°-230°. The aforementioned hydrazine hydrochloride (3 g.) is reacted with 2.6 g of 4-piperidone hydrochloride in 30 ml of ethanol saturated with gaseous HCl by heating to reflux for 2 hours. The HCl salt of 1,2,8,9,10,11-hexahydro-4H-pyrido[3',4':4,5]pyrrolo[3,2,1-jk][4,1]benzoxazepine separates out in the course of the reaction. The product was cooled, filtered, and recrystallized from ethanol. Melting point of the resulting product was 296°-297° .

Quelle