Imidazole → HCID 12151220、化合物

HRID 2415039ノート

反応式

HRID 2415039 の反応式
Cl[C:2]1[N:7]=[C:6](Cl)[C:5]([F:9])=[C:4]([C:10]([F:13])([F:12])[F:11])[N:3]=1.[NH:14]1[CH:18]=[CH:17][N:16]=[CH:15]1>C(#N)C>[F:9][C:5]1[C:6]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)=[N:7][C:2]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)=[N:3][C:4]=1[C:10]([F:13])([F:12])[F:11]

参加物

4

反応物 2

HCID 795ImidazoleHCID 133889952,4-Dichloro-5-fluoro-6-(trifluoromethyl)pyrimidine

生成物 1

HCID 12151220HCID 12151220、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2,4-Dichloro-5-fluoro-6-trifluoromethylpyrimidine (2.74 g) was dissolved in acetonitrile (30 ml) and imidazole (3.97 g) was added at room temperature with stirring. The mixture was stirred over night and then the solvent was removed under reduced pressure. The residue was added water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and brine, respectively and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was triturated with carbon tetrachloride to give crude, 5-fluoro-2,4-diimidazol-1-yl-6-trifluoromethylpyrimidine. It was recrystallized from isopropanol as colorless crystalline solid, mp 142-150° C. (decomposed).

後処理

  1. stirringThe mixture was stirred over night
  2. customthe solvent was removed under reduced pressure
  3. additionThe residue was added water
  4. extractionextracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water and brine
  6. dry with materialrespectively and dried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customThe residue was triturated with carbon tetrachloride

出典と根拠

ORDレコード
ord-39050fc2a797460ca14da09c6e6d9f03
出典データセット
uspto-grants-2004_11
特許番号
US06818631B1

反応ノート

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