Methyl 2-(triphenyl-lambda~5~-phosphanylidene)propanoate → 2-(5-chloro-3-fluoro-pyridin-2-yl)-4-methyl-5-trifluoromethyl-2H-pyridazin-3-one

HRID 840531노트

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HRID 840531 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([F:17])[C:5]([NH:8][N:9]=[CH:10][C:11](=O)[C:12]([F:15])([F:14])[F:13])=[N:6][CH:7]=1.[C:18]([C:22](=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH3:23])(OC)=[O:19]>O1CCOCC1.CCCCCC>[Cl:1][C:2]1[CH:3]=[C:4]([F:17])[C:5]([N:8]2[C:18](=[O:19])[C:22]([CH3:23])=[C:11]([C:12]([F:15])([F:14])[F:13])[CH:10]=[N:9]2)=[N:6][CH:7]=1

참가 물질

5

반응물 2

HCID 10569721Methyl 2-(triphenyl-lambda~5~-phosphanylidene)propanoateHCID 701409483-((5-Chloro-3-fluoro-pyridin-2-yl)-hydrazono)-1,1,1-trifluoropropan-2-one

생성물 1

HCID 226196692-(5-chloro-3-fluoro-pyridin-2-yl)-4-methyl-5-trifluoromethyl-2H-pyridazin-3-one

시약·촉매·용매 2

HCID 8058Hexane용매HCID 312751,4-Dioxane용매

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온도
50 °C

실험 절차

A solution of 8.09 g 3((5-chloro-3-fluoro-pyridine-2-yl) -hydrazono)-1,1,1-trifluoro-propan-2-one and 11.5 g 1-carbomethoxyethylidene triphenylphosphine in 200 ml dioxane was stired for 30 min. at 20° C. and then heated until complete conversion at 50° C. The reaction mixture was diluted with hexane, filtered from solid triphenylphosphine oxide through silicagel and evaporated. Further purification of the residue on silicagel (ethyl acetate-hexane 3:7) led to the desired product with m.p. 91-93° C.

후처리

  1. filtrationfiltered from solid triphenylphosphine oxide through silicagel
  2. customevaporated
  3. customFurther purification of the residue on silicagel (ethyl acetate-hexane 3:7)

출처 및 근거

ORD 기록
ord-b041e60a3b4b45a995bedfe6b4d41026
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06369002B1

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