3',4',5'-Trimethoxyacetophenone → 2-Bromo-1-(3,4,5-trimethoxyphenyl)ethanone

HRID 618080

反応式

HRID 618080 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13](=[O:15])[CH3:14])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].C1CNC(=O)C1.[Br:22][Br-]Br>O1CCCC1>[Br:22][CH2:14][C:13]([C:5]1[CH:6]=[C:7]([O:11][CH3:12])[C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)=[O:15]

参加物

3

反応物 1

HCID 143453',4',5'-Trimethoxyacetophenone

生成物 1

HCID 36857322-Bromo-1-(3,4,5-trimethoxyphenyl)ethanone収率 59.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

3',4',5'-Trimethoxyacetophenone (15.0 g) and pyrrolidone hydrotribromide (35.39 g) were dissolved in tetrahydrofuran (225 ml), followed by stirring at 40° C. for one hour. The reaction solution was cooled to room temperature, precipitated crystals were filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography, and the obtained crude crystals were washed with hexane (100 ml) to give 2-bromo-3',4',5'-trimethoxyacetophenone (Compound XIa, 12.20 g).

後処理

  1. temperatureThe reaction solution was cooled to room temperature
  2. customprecipitated crystals
  3. filtrationwere filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography
  6. customthe obtained crude crystals
  7. washwere washed with hexane (100 ml)

出典と根拠

ORDレコード
ord-0b230950158c4ee38d667994500d094c
出典データセット
uspto-grants-1999_09
特許番号
US05952355

関連ノート

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