Cesium carbonate → HCID 56837184、化合物

HRID 406575

反応式

HRID 406575 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:13]([CH3:14])[N:12]=[C:11]([CH3:15])[C:10]=1[NH2:16].[F:17][C:18]1[CH:19]=[C:20]([CH:23]=[C:24]([F:27])[C:25]=1F)[C:21]#[N:22].C(=O)([O-])[O-].[Cs+].[Cs+]>C(#N)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:13]([CH3:14])[N:12]=[C:11]([CH3:15])[C:10]=1[NH:16][C:25]1[C:18]([F:17])=[CH:19][C:20]([C:21]#[N:22])=[CH:23][C:24]=1[F:27]

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 5938143,4,5-TrifluorobenzonitrileHCID 66613369HCID 66613369、化合物2 回

生成物 1

HCID 56837184HCID 56837184、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
210 °C

実験手順

A mixture of 5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-1H-pyrazol-4-amin (i.e. the product of Step B) (0.25 g, 1.0 mmol), 3,4,5-trifluorobenzonitrile (0.188 g, 1.2 mmol) and cesium carbonate (0.390 g, 1.2 mmol) in acetonitrile (3 mL) was heated at 210° C. in a Biotage Initiator™ microwave apparatus for 2 h. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and filtered through a pad of silica gel on a sintered glass frit funnel. The filtrate was concentrated under reduced pressure and the resulting material was purified by silica gel chromatography (30% ethyl acetate in hexanes as eluant) to provide the title compound, a compound of the present invention, as a solid (0.065 g).

後処理

  1. temperatureAfter cooling to room temperature
  2. filtrationfiltered through a pad of silica gel on a sintered glass frit funnel
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe resulting material was purified by silica gel chromatography (30% ethyl acetate in hexanes as eluant)

出典と根拠

ORDレコード
ord-49c2671c5a1843fe8ea0eec0f1149a30
出典データセット
uspto-grants-2014_06
特許番号
US08754115B2

関連ノート

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