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Tert-Butyl hypochlorite → 4-(1-(4-Isopropyloxyphenyl)-1-methylethyl)-2-chlorophenol

HRID 260790
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HRID 260790 반응식
[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)([CH3:13])[CH3:12])=[CH:7][CH:6]=1)([CH3:3])[CH3:2].[Cl:21]OC(C)(C)C>C(Cl)(Cl)(Cl)Cl>[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[C:16]([Cl:21])[CH:15]=2)([CH3:13])[CH3:12])=[CH:7][CH:6]=1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 521297Tert-Butyl hypochloriteHCID 214662204-(1-(4-Isopropyloxyphenyl)-1-methylethyl)phenol

생성물 1

HCID 214663674-(1-(4-Isopropyloxyphenyl)-1-methylethyl)-2-chlorophenol수율 85.2%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

To a solution of 4-(1-(4-isopropyloxyphenyl)-1-methylethyl)phenol (0.51 g) in carbon tetrachloriode (1.3 ml), a solution prepared by dissolving 0.23 g of tert-butyl hypochlorite in 0.5 ml of carbon tetrachloride was added dropwise with stirring under ice cooling. After 30 minutes, an ice bath was removed, and the mixture was stirred at room temperature for 30 minutes. The reaction solution was poured into water and extracted three times with 5 ml of carbon tetrachloride. Then, the carbon tetrachloride layers were combined, washed with water, dried over anhydrous magnesium sulfate and then concentrated to give a crude product. This crude product was subjected to silica gel column chromatography to give 0.49 g of 4-(1-(4-isopropyloxyphenyl)-1-methylethyl)-2-chlorophenol (yield, 85%).

후처리

  1. additionwas added dropwise
  2. customan ice bath was removed
  3. stirringthe mixture was stirred at room temperature for 30 minutes
  4. additionThe reaction solution was poured into water
  5. extractionextracted three times with 5 ml of carbon tetrachloride
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated
  9. customto give a crude product

출처 및 근거

ORD 기록
ord-e2c8039c4f724ea49831a6906ee792a9
출처 데이터셋
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05530015

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