Sulfoxonium, trimethyl-, iodide (1:1) → 2-(2,4-Dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane

HRID 329945

반응식

HRID 329945 반응식
[I-].[CH3:2][S+](C)(C)=O.[Cl:7][C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[CH2:15][C:16]([CH3:26])([CH3:25])[C:17](=[O:24])[CH2:18][N:19]1[CH:23]=[N:22][CH:21]=[N:20]1>CS(C)=O.O1CCCC1>[Cl:7][C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[CH2:15][C:16]([C:17]1([CH2:18][N:19]2[CH:23]=[N:22][CH:21]=[N:20]2)[CH2:2][O:24]1)([CH3:26])[CH3:25]

참가 물질

5

반응물 2

HCID 74498Sulfoxonium, trimethyl-, iodide (1:1)HCID 133403824-(2,4-Dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone

생성물 1

HCID 133403832-(2,4-Dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane수율 73.7%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8028Tetrahydrofuran용매

실험 절차

15.7 g (71.2 millimoles) of trimethylsulphoxonium iodide are dissolved in 16 g of dimethylsulphoxide under a nitrogen atmosphere. 9.4 g (71.2 millimoles) of potassium tert.-butylate are added at room temperature, while cooling. The mixture is subsequently stirred for 6 hours and a solution of 20 g (64.1 millimoles) of 4-(2,4-dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanone in 30 ml of tetrahydrofuran is then added. The reaction mixture is stirred at room temperature for 15 hours and under reflux for 4 hours, cooled and poured onto water. The mixture is extracted with methylene chloride and the organic phase is dried over sodium sulphate and concentrated in vacuo. 15.4 g (73.7% of theory) of 2-(2,4-dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-yl-methyl)-oxirane of refractive index nD20 1.5539 are obtained. ##STR13##

후처리

  1. temperaturewhile cooling
  2. stirringThe reaction mixture is stirred at room temperature for 15 hours
  3. temperatureunder reflux for 4 hours
  4. temperaturecooled
  5. additionpoured onto water
  6. extractionThe mixture is extracted with methylene chloride
  7. dry with materialthe organic phase is dried over sodium sulphate
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e2278289ddc9481da80d2ae7405298b7
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04894382

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