Hydrogen Bromide → HCID 22033294, 화합물

HRID 1859338노트

반응식

HRID 1859338 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 22033294HCID 22033294, 화합물수율 96%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ec9218a9fb2e40389b1958efa2e9c0ca
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06153768

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