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

HRID 2100358노트

반응식

HRID 2100358 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 170873261-Bromo-3,5-dichloro-2-methoxybenzene수율 113.1%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e270c987cee64043a33661ecb3fdd6d6
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572797B2

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