4-Chlorophenol → HCID 13254745、化合物

HRID 569704ノート

反応式

HRID 569704 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[Na].[CH3:10][O:11][CH2:12][C:13]([C:16]1([CH2:19][N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)[CH2:18][O:17]1)([CH3:15])[CH3:14]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:18][C:16]([OH:17])([C:13]([CH3:15])([CH3:14])[CH2:12][O:11][CH3:10])[CH2:19][N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 46844-ChlorophenolHCID 5360545SodiumHCID 132547402-(Methoxy-tert.-butyl)-2-(1,2,4-triazol-1-yl-methyl)-oxirane

生成物 1

HCID 13254745HCID 13254745、化合物収率 64.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

8.1 g (0.0633 mol) of 4-chlorophenol were added to a solution of 0.32 g (0.014 mol) of sodium in 100 ml of absolute ethanol. 10.3 g (0.0488 mol) of 2-(methoxy-tert.-butyl)-2-(1,2,4-triazol-1-yl-methyl)-oxirane, dissolved in 300 ml of absolute ethanol, were added, and the reaction mixture was heated under reflux for 48 hours. The reaction mixture was allowed to cool and was concentrated. The residue was taken up in ethyl acetate, and the solution was washed once with water, once with 1N sodium hydroxide solution, again with water, thereafter with 1N hydrochloric acid and 1N sodium hydroxide solution, again with water, and finally with saturated sodium chloride solution. The organic phase was dried over sodium sulphate, and concentrated. 10.7 g (64.6% of theory) of 2-(4-chlorophenoxymethyl)-3,3-dimethyl-4-methoxy-1-(1,2,4-triazol-1-yl)-butan-2-ol of refractive index nD20 =1.531 were obtained.

後処理

  1. additionwere added
  2. temperaturethe reaction mixture was heated
  3. temperatureunder reflux for 48 hours
  4. temperatureto cool
  5. concentrationwas concentrated
  6. washthe solution was washed once with water, once with 1N sodium hydroxide solution, again with water
  7. dry with materialThe organic phase was dried over sodium sulphate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-b095ca6a6dc5488fb1793341f859723b
出典データセット
uspto-grants-1988_03
特許番号
US04734126

反応ノート

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