Potassium Hydroxide → 3-Bromo-4-methoxyphenol

HRID 2097589노트

반응식

HRID 2097589 반응식
[OH-].[K+].[Br:3][C:4]1[CH:5]=[C:6]([O:12]C(=O)C)[CH:7]=[CH:8][C:9]=1[O:10][CH3:11]>O.CO>[Br:3][C:4]1[CH:5]=[C:6]([OH:12])[CH:7]=[CH:8][C:9]=1[O:10][CH3:11]

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 145058743-Bromo-4-methoxyphenyl acetate

생성물 1

HCID 6088153-Bromo-4-methoxyphenol수율 98.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A solution of potassium hydroxide (290 mg, 5.19 mmol) in water (2.5 mL) was added to a solution of acetic acid 3-bromo-4-methoxy-phenyl ester (1.2 g, 4.9 mmol) in methanol (18.5 mL). Mixture was stirred at ambient temperature for 30 min, then solvents were removed in vacuo and water (40 mL) added. The mixture was made acidic by drop-wise addition of 1.2 M aq HCl solution (4.3 mL) and the mixture extracted with dichloromethane (2×40 mL). Combined organics were dried over sodium sulphate, filtered and filtrate solvents evaporated in vacuo to give the title compound (976 mg, 98%) as a pale yellow solid.

후처리

  1. customsolvents were removed in vacuo and water (40 mL)
  2. additionadded
  3. additionThe mixture was made acidic by drop-wise addition of 1.2 M aq HCl solution (4.3 mL)
  4. extractionthe mixture extracted with dichloromethane (2×40 mL)
  5. dry with materialCombined organics were dried over sodium sulphate
  6. filtrationfiltered
  7. customfiltrate solvents evaporated in vacuo

출처 및 근거

ORD 기록
ord-cb11fefe9fa3490cb62d5b568c6c1ffd
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450346B2

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