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

HRID 260790
ノート
印刷プレビュー

反応式

HRID 260790 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-e2c8039c4f724ea49831a6906ee792a9
出典データセット
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05530015

反応ノート

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