Trifluoroacetic acid → 1-[2-fluoro-4-(1H-pyrazol-1-yl)phenyl]-5-methoxy-3-[1-(2,2,2-trifluoroethyl)-1H-pyrazol-5-yl]pyridazin-4(1H)-one

HRID 1528047ノート

反応式

HRID 1528047 の反応式
CN(C)[CH:3]=[CH:4][C:5]([C:7]1[C:12](=[O:13])[C:11]([O:14][CH3:15])=[CH:10][N:9]([C:16]2[CH:21]=[CH:20][C:19]([N:22]3[CH:26]=[CH:25][CH:24]=[N:23]3)=[CH:18][C:17]=2[F:27])[N:8]=1)=O.[F:29][C:30]([F:35])([F:34])[CH2:31][NH:32][NH2:33].C(O)(C(F)(F)F)=O>C(O)C>[F:27][C:17]1[CH:18]=[C:19]([N:22]2[CH:26]=[CH:25][CH:24]=[N:23]2)[CH:20]=[CH:21][C:16]=1[N:9]1[CH:10]=[C:11]([O:14][CH3:15])[C:12](=[O:13])[C:7]([C:5]2[N:32]([CH2:31][C:30]([F:35])([F:34])[F:29])[N:33]=[CH:3][CH:4]=2)=[N:8]1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 787402,2,2-TrifluoroethylhydrazineHCID 712721203-[3-(dimethylamino)prop-2-enoyl]-1-[2-fluoro-4-(1H-pyrazol-1-yl)phenyl]-5-methoxypyridazin-4(1H)-one

生成物 1

HCID 680146991-[2-fluoro-4-(1H-pyrazol-1-yl)phenyl]-5-methoxy-3-[1-(2,2,2-trifluoroethyl)-1H-pyrazol-5-yl]pyridazin-4(1H)-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a suspension of 3-[3-(dimethylamino)prop-2-enoyl]-5-methoxy-1-[2-fluoro-4-(1H-pyrazol-1-yl)phenyl]pyridazin-4(1H)-one (200 mg) in ethanol (2.0 mL) was added dropwise a solution of 2,2,2-trifluoroethylhydrazine (0.0483 mL) and TFA (0.2 mL) in ethanol (2.0 mL), and the mixture was stirred at room temperature for 48 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (170 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-328bf34156b14349806097335ac37e5c
出典データセット
uspto-grants-2015_07
特許番号
US09090586B2

反応ノート

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