Pyridine → 4-Bromo-2-fluorophenyl acetate

HRID 38997

反応式

HRID 38997 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 226485254-Bromo-2-fluorophenyl acetate収率 83%

反応条件

温度
100 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0ee4864d93714b428fe4be10c94032b6
出典データセット
uspto-grants-2013_09
特許番号
US08524766B2

関連ノート

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