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2,4-Dichlorophenol → 1-(2,4-Dichlorophenoxy)-3,3-dimethyl-4-fluoro-2-butanone

HRID 904648
ノート
印刷プレビュー

反応式

HRID 904648 の反応式
Br[CH2:2][C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][F:6].C(=O)([O-])[O-].[K+].[K+].[Cl:16][C:17]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:18]=1[OH:24]>CC(C)=O>[Cl:16][C:17]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:18]=1[O:24][CH2:2][C:3](=[O:9])[C:4]([CH3:8])([CH3:7])[CH2:5][F:6]
参加物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 84492,4-DichlorophenolHCID 11430Potassium CarbonateHCID 130194421-Bromo-3,3-dimethyl-4-fluoro-2-butanone

生成物 1

HCID 130194431-(2,4-Dichlorophenoxy)-3,3-dimethyl-4-fluoro-2-butanone収率 88%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

A solution of 197 g (1 mol) of 1-bromo-3,3-dimethyl-4-fluoro-2-butanone in 100 ml of acetone was added dropwise, at the boiling point, to 140 g (1 mol) of potassium carbonate and 163 g (1 mol) of 2,4-dichlorophenol in 1,000 ml of acetone. The mixture was stirred under reflux for 20 hours, cooled and filtered. The filtrate was concentrated by distilling off the acetone under a waterpump vacuum. The residue was dissolved in 500 ml of toluene, washed with 500 ml of 10% strength sodium hydroxide solution and with two 250 ml portions of water, dried over sodium sulphate and concentrated by distilling off the toluene under a waterpump vacuum. 244.6 g (88% of theory) of 1-(2,4-dichlorophenoxy)-3,3-dimethyl-4-fluoro-2-butanone were obtained as a highly viscous oil which could be further reacted in crude form.

後処理

  1. temperatureunder reflux for 20 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated
  5. distillationby distilling off the acetone under a waterpump vacuum
  6. dissolutionThe residue was dissolved in 500 ml of toluene
  7. washwashed with 500 ml of 10% strength sodium hydroxide solution and with two 250 ml portions of water
  8. dry with materialdried over sodium sulphate
  9. concentrationconcentrated
  10. distillationby distilling off the toluene under a waterpump vacuum

出典と根拠

ORDレコード
ord-863e67b5e218485582c81e7b30d607c0
出典データセット
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04419361

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