Climbazole → 1-(4-Chlorophenoxy)-1-(1H-imidazol-1-yl)-3,3-dimethylbutan-2-ol

HRID 1758081

반응식

HRID 1758081 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH:7]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)[C:8](=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][CH:3]=1.C(O)=O.C(N(CC)CC)C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH:7]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)[CH:8]([OH:13])[C:9]([CH3:11])([CH3:12])[CH3:10])=[CH:19][CH:20]=1

참가 물질

3

반응물 2

HCID 37907ClimbazoleHCID 11084032Triethylammonium formate

생성물 1

HCID 1714401-(4-Chlorophenoxy)-1-(1H-imidazol-1-yl)-3,3-dimethylbutan-2-ol수율 56%

실험 절차

14 g (0.048 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-one and 61.8 g (0.143 mol) of formic acid/triethylamine (5:2 addition compound) were heated at 145° C. for 4 hours. The reaction mixture was allowed to cool and was concentrated in vacuo. The residue was taken up in dilute sodium hydroxide solution and the mixture was extracted with methylene chloride. The organic phase was washed with water, dried over sodium sulphate and concentrated in vacuo. The residue was suspended in hot cyclohexane, the suspension was filtered hot and the solid was dried. 7.9 g (56% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-ol of melting point 145°-147° C. were obtained.

후처리

  1. temperatureto cool
  2. concentrationwas concentrated in vacuo
  3. extractionthe mixture was extracted with methylene chloride
  4. washThe organic phase was washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo
  7. filtrationthe suspension was filtered hot
  8. customthe solid was dried

출처 및 근거

ORD 기록
ord-02f111901faa45cf844be6429bc0bf42
출처 데이터셋
uspto-grants-1983_02
특허 번호
US04371700

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