Water → 6-(4-Bromophenyl)-3-(2,6-difluorophenyl)-[1,2,4]triazine

HRID 2085918ノート

反応式

HRID 2085918 の反応式
C(OC([NH:8][NH:9][C:10]([C:12]1[C:17]([F:18])=[CH:16][CH:15]=[CH:14][C:13]=1[F:19])=N)=O)(C)(C)C.[Br:20][C:21]1[CH:26]=[CH:25][C:24]([C:27](=O)[CH:28]=[N:29]O)=[CH:23][CH:22]=1.C([O-])(=O)C.[Na+].O>C(O)(=O)C>[Br:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[N:8]=[N:9][C:10]([C:12]3[C:13]([F:19])=[CH:14][CH:15]=[CH:16][C:17]=3[F:18])=[N:29][CH:28]=2)=[CH:23][CH:22]=1

参加物

6

反応物 4

HCID 962WaterHCID 517045Sodium AcetateHCID 72814957(4-Bromo-phenyl)-oxo-acetaldehyde oximeHCID 178454364HCID 178454364、化合物

生成物 1

HCID 227270186-(4-Bromophenyl)-3-(2,6-difluorophenyl)-[1,2,4]triazine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
10 °C

実験手順

A mixture of 200 mg of N′-[(2,6-difluorophenyl)-iminomethyl]-hydrazinecarboxylic acid tert-butyl ester, 114 mg of (4-bromophenyl)-oxoacetaldehyde oxime and 123 mg of sodium acetate in 1.5 ml of glacial acetic acid is heated at 10° C. for 3 h. After cooling to room temperature, the reaction mixture is poured into water and extracted with ethyl acetate. The organic phase is washed in succession with saturated sodium hydrogen carbonate solution and saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated. The residue is purified by means of flash chromatography (1% methanol in dichloromethane). In this way the title compound having a melting point of 180-181° C. is obtained.

後処理

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is washed in succession with saturated sodium hydrogen carbonate solution and saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue is purified by means of flash chromatography (1% methanol in dichloromethane)
  8. customis obtained

出典と根拠

ORDレコード
ord-752c34a7b7354a6fa46ce6e7d9bcd369
出典データセット
uspto-grants-2004_04
特許番号
US06723720B2

反応ノート

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