Pyridine → 4-Bromo-2-fluorophenyl acetate

HRID 38997

반응식

HRID 38997 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([F:9])[CH:3]=1.[C:10](OC(=O)C)(=[O:12])[CH3:11].N1C=CC=CC=1>>[C:10]([O:8][C:5]1[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=1[F:9])(=[O:12])[CH3:11]

참가 물질

4

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 27249814-Bromo-2-fluorophenol

생성물 1

HCID 226485254-Bromo-2-fluorophenyl acetate수율 83%

반응 조건

온도
100 °C

실험 절차

A mixture of 4-bromo-2-fluorophenol (5 g, 30 mmol) and acetic anhydride (13.4 g, 130 mmol) in pyridine (10.6 ml, 130 mmol) was heated at 100° C. for 3 h and then brought to ambient temperature and poured into water. HCl (1 N and 6 N) was added and the solution was extracted with EtOAc. The combined organic phases were washed with sodium bicarbonate (saturated, 3×50 ml), dried (Na2SO4) and evaporated to dryness to give the title compound (5.8 g). MS m/z (rel. intensity, 70 eV) 233 (M+, 11), 232 (M+, 12), 191 (95), 190 (bp), 161 (8).

후처리

  1. custombrought to ambient temperature
  2. additionwas added
  3. extractionthe solution was extracted with EtOAc
  4. washThe combined organic phases were washed with sodium bicarbonate (saturated, 3×50 ml)
  5. dry with materialdried (Na2SO4)
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-0ee4864d93714b428fe4be10c94032b6
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524766B2

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