Реакция #81798

Уравнение реакции

hexane

Ethylamine

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

→

title compound

Выход 76.2%

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

Выход 76.2%

Растворители

xylene

ethyl acetate

Условия реакции

Обработка

1. 1
   ДругоеThe solvent was removed in vacuo and water
2. 2
   workup.ADDITIONadded to the residue
3. 3
   ЭкстракцияThe product was extracted with ether
4. 4
   Сушкаdried (sodium sulfate)
5. 5
   Концентрированиеconcentrated
6. 6
   Другоеto give an oil
7. 7
   Другоеformed
8. 8
   ФильтрацияThe solid was filtered
9. 9
   Другоеdried

Методика

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.

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