Reaktion #215828

Reaktionsgleichung

8-chlorodibenz[b,f][1,41oxazepine-10(11H)-carboxylic acid, 2-[1-oxo-3-(2-pyridinyl)propyl]hydrazide

→

white powder

Ausbeute 153.4%

8-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, 2-[1-oxo-3-(2-pyridinyl)propyl]hydrazide, monohydrochloride

Ausbeute 153.4%

Lösungsmittel

—

3A

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationfiltered
2. 2
   Sonstigeto remove any undissolved material
3. 3
   TemperaturThe solution was cooled in an ice bath
4. 4
   workup.ADDITIONTo this was added dropwise 5.3 mL of 9.5M hydrogen chloride in ethanol
5. 5
   workup.STIRRINGAfter stirring in the ice bath for 5 minutes
6. 6
   Sonstigesome of the product precipitated
7. 7
   workup.ADDITIONThis was poured slowly into 275 mL of stirring diethyl ether (Et2O)
8. 8
   workup.STIRRINGthe resulting mixture was stirred for 5 minutes
9. 9
   FiltrationThe resulting solid product was collected by filtration
10. 10
    Waschenwashed with 20 mL of 3A ethanol
11. 11
    Sonstigedried under vacuum at 56° C.

Vorschrift

2.64 g of 8-chlorodibenz[b,f][1,41oxazepine-10(11H)-carboxylic acid, 2-[1-oxo-3-(2-pyridinyl)propyl]hydrazide (6), prepared as described above in Example 6, was taken up in 25 mL of 3A ethanol and filtered to remove any undissolved material. The solution was cooled in an ice bath with stirring. To this was added dropwise 5.3 mL of 9.5M hydrogen chloride in ethanol. After stirring in the ice bath for 5 minutes, some of the product precipitated. This was poured slowly into 275 mL of stirring diethyl ether (Et2O), and the resulting mixture was stirred for 5 minutes. The resulting solid product was collected by filtration, washed with 20 mL of 3A ethanol, followed by Et2O, and dried under vacuum at 56° C. to yield 2.20 g (76.7%) of a white powder. Analysis calculated for C22H20N4O3Cl2 : C, 57.53; H, 4.39; N, 12.20; C1, 15.44; Found: C, 57.31; H, 4.36; N, 11.98; Cl, 15.11.

Quelle