Water → 2-(2,4-Dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane

HRID 979457ノート

反応式

HRID 979457 の反応式
[I-].[CH3:2][S+](C)C.[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[CH2:14][C:15]([CH3:25])([CH3:24])[C:16](=[O:23])[CH2:17][N:18]1[CH:22]=[N:21][CH:20]=[N:19]1.O>CS(C)=O.O1CCCC1>[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[CH2:14][C:15]([C:16]1([CH2:17][N:18]2[CH:22]=[N:21][CH:20]=[N:19]2)[CH2:2][O:23]1)([CH3:25])[CH3:24]

参加物

6

反応物 3

HCID 962WaterHCID 75127Trimethylsulfonium iodideHCID 133403824-(2,4-Dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone

生成物 1

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

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

15.7 g (71.2 mmol) of trimethylsulphonium iodide are dissolved in 16 g of dimethyl sulphoxide under an atmosphere of nitrogen. 9.4 g (71.2 mmol) of potassium tert.-butylate are added at room temperature, with cooling. The mixture is allowed to stir for 6 hours and then a solution of 20 g (64.1 mmol) of 4-(2,4-dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone in 30 ml of tetrahydrofuran is added. The reaction mixture is allowed to stir at room temperature for 15 hours and under reflux for 4 hours, then cooled and poured into water. The mixture is extracted with methylene chloride, and the organic phase is dried over sodium sulphate and evaporated in vacuo. 15.4 g (73.7% of theory) of 2-(2,4-dichlorophenyl-tert.-butyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane of refractive index nD20 =1.5539 are obtained. ##STR95##

後処理

  1. temperaturewith cooling
  2. stirringto stir at room temperature for 15 hours
  3. temperatureunder reflux for 4 hours
  4. temperaturecooled
  5. extractionThe mixture is extracted with methylene chloride
  6. dry with materialthe organic phase is dried over sodium sulphate
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-9a9f9b6385914f5cb7f5ab62620665d3
出典データセット
uspto-grants-1987_05
特許番号
US04668660

反応ノート

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