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

HRID 618080

반응식

HRID 618080 반응식
[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]

참가 물질

3

반응물 1

HCID 143453',4',5'-Trimethoxyacetophenone

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-0b230950158c4ee38d667994500d094c
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952355

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