Acetic Acid → 2-Fluoro-5-methoxybenzoic acid

HRID 265002

반응식

HRID 265002 반응식
[F:1][C:2]1C=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1C.Br.O=O.[C:14]([OH:17])(=[O:16])[CH3:15]>O.O.O.O.C([O-])(=O)C.[Co+2].C([O-])(=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH3:9])=[CH:6][C:15]=1[C:14]([OH:17])=[O:16]

참가 물질

6

반응물 4

HCID 176Acetic Acid2회HCID 260Hydrogen BromideHCID 977OxygenHCID 1375464-Fluoro-3-methylanisole

생성물 1

HCID 27745432-Fluoro-5-methoxybenzoic acid

시약·촉매·용매 1

HCID 61372Cobalt(II) acetate tetrahydrate촉매

실험 절차

The title compound was prepared according to a method reported by Hay and Blanchard [Canad. J. Chem. 43, 1306 (1965)]. In a three-necked round-bottom flask (1000 mL), equipped with a magnetic stirrer, thermometer, reflux condensor and a gas distribution tube, cobalt(II)acetate tetrahydrate (12.6 g; 51 mmol) was dissolved in glacial acetic acid (404 mL) by stirring. Commercial 4-fluoro-3-methylanisole (35.4, 252 mmol) and 33% HBr in acetic acid (10.1 mL; 51 mmol) were added and then the mixture was heated on an oil-bath to 90°-95° C. All the time a stream of oxygen was passed through the solution at a rate of about 660 mL/min. After 3 hours the reaction mixture was cooled to room temperature and then rotary evaporated to dryness.

후처리

  1. customIn a three-necked round-bottom flask (1000 mL), equipped with a magnetic stirrer
  2. temperaturethe mixture was heated on an oil-bath to 90°-95° C
  3. customrotary evaporated to dryness

출처 및 근거

ORD 기록
ord-673cebf161634791b7ae93b780a22b98
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646309

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