반응 #215830

반응 방정식

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

용매

acetic acid

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후처리

1. 1
   기타prepared
2. 2
   여과filtered
3. 3
   workup.ADDITIONTo the filtrate was added 5 mL of 6N HCl dioxane
4. 4
   기타The hydrochloride salt was precipitated from the reaction by the addition of Et2O
5. 5
   여과The resultant solid product was collected by filtration
6. 6
   기타dried in an Abderhalden
7. 7
   기타drying pistol

실험 절차

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.

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