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Carbon Tetrachloride → 3-Tert-butyl-4-chlorophenol

HRID 979718
ノート
印刷プレビュー

反応式

HRID 979718 の反応式
[C:1]([Cl:5])(Cl)(Cl)Cl.[C:6]([C:10]1[CH:11]=[C:12]([OH:16])[CH:13]=[CH:14]C=1)([CH3:9])([CH3:8])[CH3:7].S(Cl)(Cl)(=O)=O>O>[C:6]([C:10]1[CH:11]=[C:12]([OH:16])[CH:13]=[CH:14][C:1]=1[Cl:5])([CH3:9])([CH3:8])[CH3:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5943Carbon TetrachlorideHCID 11450Phenol, 3-(1,1-dimethylethyl)-HCID 24648Sulfuryl chloride

生成物 1

HCID 109102303-Tert-butyl-4-chlorophenol

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

Into 30 ml of carbon tetrachloride were dissolved 9 g of 3-tert-butylphenol and the mixture was heated up to 70° C. With stirring at this temperature, 10.5 g of sulfuryl chloride were added dropwise to the mixture. After completion of this dropwise addition, the reaction mixture was subjected to stirring over a period of 48 hours at 70° C. After cooling the reaction mixture down to room temperature, the reaction mixture was poured into cold water and the resultant product was extracted with carbon tetrachloride. After drying over anhydrous calcium chloride, carbon tetrachloride of the extraction solution was distilled off under reduced pressure, and the residue was purified through a column chromatography (employing silica gel as carrier and benzene as developing solvent) to give 1.3 g of 3-tert-butyl-4-chlorophenol, having the following properties.

後処理

  1. additionwere added dropwise to the mixture
  2. additionAfter completion of this dropwise addition
  3. temperatureAfter cooling the reaction mixture down to room temperature
  4. extractionthe resultant product was extracted with carbon tetrachloride
  5. dry with materialAfter drying over anhydrous calcium chloride, carbon tetrachloride of the extraction solution
  6. distillationwas distilled off under reduced pressure
  7. customthe residue was purified through a column chromatography (employing silica gel as carrier and benzene as developing solvent)

出典と根拠

ORDレコード
ord-ebddf4854b584d03bb16867318282229
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04668831

反応ノート

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