Potassium Carbonate → 5'-Chloro-2'-(2-methyl-2-propenyloxy)acetophenone

HRID 416025

反応式

HRID 416025 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][C:20]([CH3:22])=[CH2:21]>CN(C)C=O.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:21][C:20]([CH3:22])=[CH2:19])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 740613-Chloro-6-hydroxyacetophenoneHCID 3577853-Bromo-2-methyl-1-propene

生成物 1

HCID 582940385'-Chloro-2'-(2-methyl-2-propenyloxy)acetophenone収率 97.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A suspension of 5′-chloro-2′-hydroxyacetophenone (0.86 g, 5.0 mmol), potassium carbonate (1.4 g, 10 mmol) and 3-bromo-2-methylpropene (0.56 mL, 5.5 mmol) in anhydrous N,N-dimethylformamide (20 mL) was stirred at 60° C. for 4 hours. After cooling, the reaction mixture was diluted with water (100 mL), and the whole was extracted with ethyl acetate (100 mL). The organic layer was washed with saturated aqueous ammonium chloride solution (50 mL) and brine (50 mL) and dried over anhydrous magnesium sulfate. The solvent was removed in vacuo to give the title reference compound (1.1 g) as orange oil (Yield 96%).

後処理

  1. temperatureAfter cooling
  2. extractionthe whole was extracted with ethyl acetate (100 mL)
  3. washThe organic layer was washed with saturated aqueous ammonium chloride solution (50 mL) and brine (50 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-1609479122814f759c812f9af7a87ca2
出典データセット
uspto-grants-2012_01
特許番号
US08088817B2

関連ノート

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