Acetonitrile → 1-Phenyl-2-(1H-1,2,4-triazol-1-yl)propan-1-one

HRID 2166354노트

반응식

HRID 2166354 반응식
Br[CH:2]([CH3:11])[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].N1C=[CH:15][N:14]=[N:13]1.[C:17](#[N:19])C>>[N:14]1([CH:2]([CH3:11])[C:3]([C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)=[O:4])[CH:15]=[N:19][CH:17]=[N:13]1

참가 물질

4

반응물 3

HCID 6342Acetonitrile2회HCID 164522-BromopropiophenoneHCID 178418936HCID 178418936, 화합물

생성물 1

HCID 132599821-Phenyl-2-(1H-1,2,4-triazol-1-yl)propan-1-one수율 55%

실험 절차

To a solution of 223 g (1 mol) of 2-bromopropiophenone in 300 ml of acetonitrile is added dropwise to a boiling mixture of 414 g (6 mols) of triazole and 1,200 ml of acetonitrile, and the mixture is heated at the boil for 8 hours. Thereafter, the mixture is evaporated down in vacuo, the residue is taken up in 750 ml of dichloromethane and 750 ml of water, and the organic phase is washed with several 500 ml portions of water and dried over anhydrous sodium sulphate. After the solvent has been distilled off, the remaining residue is distilled in vacuo. 111 g (55% of theory) of 2-(1,2,4-triazol-1-yl)-propiophenone of boiling point 133° C./0.15 mbar and of melting point 117° C. are obtained. ##STR21##

후처리

  1. temperaturethe mixture is heated at the boil for 8 hours
  2. customThereafter, the mixture is evaporated down in vacuo
  3. wash750 ml of water, and the organic phase is washed with several 500 ml portions of water
  4. dry with materialdried over anhydrous sodium sulphate
  5. distillationAfter the solvent has been distilled off
  6. distillationthe remaining residue is distilled in vacuo

출처 및 근거

ORD 기록
ord-17777ef263d142faaeb1af6a7600d4ae
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04945101

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