Hydrogen Bromide → HCID 22033294、化合物

HRID 1859338ノート

反応式

HRID 1859338 の反応式
C[O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:22])[C:8]([C:14]3[CH:19]=[CH:18][C:17]([O:20]C)=[CH:16][CH:15]=3)([CH3:13])[CH2:9][S:10]2)=[CH:5][CH:4]=1.Br>C(O)(=O)C>[OH:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:22])[C:8]([C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=3)([CH3:13])[CH2:9][S:10]2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 109799547-Methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one

生成物 1

HCID 22033294HCID 22033294、化合物収率 96%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To acetic acid solution (15 ml) of 7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one (2.82 g, 8.99 mmol) was added aqueous 48% HBr solution (13 ml) and the mixture was heated under refluxing for 24 hours. The reaction solution was extracted with ethyl acetate, and the organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated saline, dried over anhydrous magnesium sulfate and then distilled under reduced pressure to remove the solvent. The crude product thus obtained was purified with silica gel column chromatography (ethyl acetate:hexane=2:1) to obtain 2.46 g (yield: 96%) of the title compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder refluxing for 24 hours
  3. extractionThe reaction solution was extracted with ethyl acetate
  4. washthe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated saline
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationdistilled under reduced pressure
  7. customto remove the solvent
  8. customThe crude product thus obtained
  9. customwas purified with silica gel column chromatography (ethyl acetate:hexane=2:1)

出典と根拠

ORDレコード
ord-ec9218a9fb2e40389b1958efa2e9c0ca
出典データセット
uspto-grants-2000_11
特許番号
US06153768

反応ノート

読み込み中…