Hydrochloric Acid → 1-Bromo-3,5-dichloro-2-methoxybenzene

HRID 2100358ノート

反応式

HRID 2100358 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[OH:10].[C:11](=O)([O-])[O-].[K+].[K+].CI.Cl>CC(C)=O>[Br:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[O:10][CH3:11]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 206172-Bromo-4,6-dichlorophenol

生成物 1

HCID 170873261-Bromo-3,5-dichloro-2-methoxybenzene収率 113.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
0 °C

実験手順

2-Bromo-4,6-dichlorophenol (Preparation 24, 4.6 g, 19 mmol), potassium carbonate (4.5 g, 32.3 mmol) and methyl iodide (1.8 ml, 20.5 mmol) were combined in 46 ml acetone and heated to reflux for 18 hours. The reaction was cooled to 0° C., 1N HCl (aqueous) was added to give pH 3, and the reaction was extracted into 50 ml ethyl acetate. The organic layer was washed with brine (2×20 ml), dried over sodium sulphate and concentrated in vacuo to afford the title compound as a brown solid (5.5 g).

後処理

  1. temperatureheated
  2. temperatureto reflux for 18 hours
  3. customto give pH 3
  4. extractionthe reaction was extracted into 50 ml ethyl acetate
  5. washThe organic layer was washed with brine (2×20 ml)
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e270c987cee64043a33661ecb3fdd6d6
出典データセット
uspto-grants-2009_08
特許番号
US07572797B2

反応ノート

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