Reaktion #215830

Reaktionsgleichung

8-chlorodibenz[b,f][1,41oxazepine-10(11H)-carboxylic acid, hydrazide

3-(3-pyridyl)propionic acid

→

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

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   Filtrationfiltered
3. 3
   workup.ADDITIONTo the filtrate was added 5 mL of 6N HCl dioxane
4. 4
   SonstigeThe hydrochloride salt was precipitated from the reaction by the addition of Et2O
5. 5
   FiltrationThe resultant solid product was collected by filtration
6. 6
   Sonstigedried in an Abderhalden
7. 7
   Sonstigedrying pistol

Vorschrift

The experiment described above in Example 7 was repeated on a five mmol scale with 8-chlorodibenz[b,f][1,41oxazepine-10(11H)-carboxylic acid, hydrazide (1), prepared as described above in Example 1, and 3-(3-pyridyl)propionic acid. The yield of the reaction product was 0.75 g (34%). The free base was dissolved in 5 mL of acetic acid (HOAc) and filtered. To the filtrate was added 5 mL of 6N HCl dioxane. The hydrochloride salt was precipitated from the reaction by the addition of Et2O. The resultant solid product was collected by filtration and dried in an Abderhalden drying pistol. Analysis calculated for C22H20N4O3Cl2 : C, 57.53; H, 4.39; N, 12.20; Cl, 15.44. Found: C, 57.35; H, 4.45; N, 12.08; Cl, 15.58.

Quelle