2,4-Dichlorophenol → HCID 23349979、化合物

HRID 2058195ノート

反応式

HRID 2058195 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[OH:9].Br[CH2:11][C:12](=[O:18])[C:13]([O:16][CH3:17])([CH3:15])[CH3:14].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[O:9][CH2:11][C:12](=[O:18])[C:13]([O:16][CH3:17])([CH3:15])[CH3:14]

参加物

5

反応物 3

HCID 84492,4-DichlorophenolHCID 11430Potassium CarbonateHCID 1278370276336-55-5

生成物 1

HCID 23349979HCID 23349979、化合物収率 85.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
-20 °C

実験手順

A stirred mixture of 13.04 g (0.08 mole) of 2,4-dichlorophenol, 15.61 g (0.08 mole) 1-bromo-3-methoxy-3-methyl-2-butanone, and 11.1 g (0.08 mole) powdered potassium carbonate in 300 ml acetonitrile was heated at reflux temperature for 30 minutes. The reaction mixture was cooled, filtered, and the solvent evaporated from the filtrate. The residual oil was taken up in hexane and cooled to -20° C., whereupon the product separated as a white crystalline solid. There was thus obtained 19 g (85.7% yield) of 1-(2,4-dichlorophenoxy)-3-methoxy-3-methyl-2-butanone, m.p. 45.5°-47.5° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 30 minutes
  3. temperatureThe reaction mixture was cooled
  4. filtrationfiltered
  5. customthe solvent evaporated from the filtrate
  6. customseparated as a white crystalline solid

出典と根拠

ORDレコード
ord-94e719e0b8644da6af17b1cdb3e70968
出典データセット
uspto-grants-1980_07
特許番号
US04215127

反応ノート

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