반응 #41777

반응 방정식

(3-chlorophenyl)-N-methylcarboxamide

potassium carbonate

2-methoxy-4-(methylamino)-5-nitrophenol

potassium-t-butoxide

N,N-dimethylacetamide

→

{4-[2-methoxy-4-(methylamino)-5-nitrophenoxy](2-pyridyl)}-N-methylcarboxamide

반응 조건

후처리

1. 1
   온도It was then heated to 110° C. for 12 h
2. 2
   온도After cooling to ambient temperature the solvent
3. 3
   workup.DISTILLATIONwas distilled off
4. 4
   추출the resulting solid was extracted
5. 5
   기타for 48 h
6. 6
   온도The organic layer was cooled to 0° C.
7. 7
   기타when the product crystallized from the ethyl acetate

실험 절차

To a stirred solution of 2-methoxy-4-(methylamino)-5-nitrophenol (1 eq) in N,N-dimethylacetamide was added potassium-t-butoxide (1.2 eq) and continued stirring at ambient temperature utility solidified. To it was then added (3-chlorophenyl)-N-methylcarboxamide (1 eq) and anhydrous potassium carbonate (1 eq) and the resulting mixture was heated to 50° C. whereby the solid liquified. It was then heated to 110° C. for 12 h. After cooling to ambient temperature the solvent was distilled off and the resulting solid was extracted using ethyl acetate in a soxhlet apparatus for 48 h. The organic layer was cooled to 0° C., when the product crystallized from the ethyl acetate to give {4-[2-methoxy-4-(methylamino)-5-nitrophenoxy](2-pyridyl)}-N-methylcarboxamide. MS: MH+ 332

출처