반응 #81798

반응 방정식

hexane

Ethylamine

2-chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide

→

title compound

수율 76.2%

N-(2-Chloro-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide

수율 76.2%

용매

xylene

ethyl acetate

반응 조건

후처리

1. 1
   기타The solvent was removed in vacuo and water
2. 2
   workup.ADDITIONadded to the residue
3. 3
   추출The product was extracted with ether
4. 4
   건조dried (sodium sulfate)
5. 5
   농축concentrated
6. 6
   기타to give an oil
7. 7
   기타formed
8. 8
   여과The solid was filtered
9. 9
   기타dried

실험 절차

Ethylamine (12.7 g) was added to a suspension of 21.0 g of the 2-chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide in 150 ml of xylene in a steel bomb. The mixture was then heated in an oil bath to 165° C. for 6 hrs. and then stirred overnight at room temperature. The solvent was removed in vacuo and water added to the residue. The product was extracted with ether, dried (sodium sulfate) and concentrated to give an oil. This was dissolved in ethyl acetate followed by hexane at which time a precipitate formed. The solid was filtered and dried to give 16.5 g of the title compound, m.p. 122°-124° C.

출처