4-Chlorophenol → HCID 13254745、化合物

HRID 2291715ノート

反応式

HRID 2291715 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, dissolve 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-fe7ae77932944af1ba22b44353aafca2
出典データセット
uspto-grants-1989_01
特許番号
US04797499

反応ノート

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