Water → 1-(2-Fluoro-5-methoxybenzylidene)-2-(4-fluorophenyl)hydrazine

HRID 13187

反応式

HRID 13187 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1.[F:10][C:11]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:12]=1[CH:13]=O.C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C=O)C>[F:10][C:11]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:12]=1[CH:13]=[N:9][NH:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1

参加物

6

反応物 4

HCID 962WaterHCID 10796Cesium carbonateHCID 69982(4-Fluorophenyl)hydrazineHCID 27348722-Fluoro-5-methoxybenzaldehyde

生成物 1

HCID 668125981-(2-Fluoro-5-methoxybenzylidene)-2-(4-fluorophenyl)hydrazine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

(4-fluorophenyl)hydrazine (6.5 g, 40 mmol), 2-fluoro-5-methoxybenzaldehyde (6.2 g, 40 mmol) and cesium carbonate (13 g, 40 mmol) were stirred in DMF (40 mL) at r.t. under argon atmosphere for 1.5 h and was then poured with stirring into water and extracted with ethyl acetate. The organic phase was washed trice with water, then brine and evaporated. The residue crystallized slowly to afford the subtitle compound as a beige-light brown crystal mass (10.21 g).

後処理

  1. additionwas then poured
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed trice with water
  4. custombrine and evaporated
  5. customThe residue crystallized slowly

出典と根拠

ORDレコード
ord-5de05775b2444b41b706539db408683e
出典データセット
uspto-grants-2010_06
特許番号
US07728030B2

関連ノート

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