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

HRID 979718
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HRID 979718 반응식
[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]
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참가 물질

5

반응물 3

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

생성물 1

HCID 109102303-Tert-butyl-4-chlorophenol

시약·촉매·용매 1

HCID 962Water용매

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온도
70 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ebddf4854b584d03bb16867318282229
출처 데이터셋
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04668831

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