Imidazole → HCID 12151220, 화합물

HRID 2415039노트

반응식

HRID 2415039 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 12151220HCID 12151220, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-39050fc2a797460ca14da09c6e6d9f03
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06818631B1

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