Water → 4'-Bromo-4-carboxymethylbiphenyl

HRID 1004515

반응식

HRID 1004515 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11](C(=O)C)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[S].[OH2:18].N1[CH2:24][CH2:23][O:22]CC1>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH2:24][C:23]([OH:22])=[O:18])=[CH:10][CH:9]=2)=[CH:6][CH:7]=1

참가 물질

5

반응물 4

HCID 962WaterHCID 8083MorpholineHCID 798061-(4'-Bromo(1,1'-biphenyl)-4-yl)ethan-1-oneHCID 5362487Sulfur

생성물 1

HCID 13942454'-Bromo-4-carboxymethylbiphenyl

실험 절차

The compound (3 g) obtained in the above (1) is suspended in morpholine (20 ml), and thereto is added sulfur (0.71 g), and the mixture is refluxed with stirring for five hours. After cooling, the reaction mixture is poured into water, and extracted with ethyl acetate. The organic layer is washed with 1N hydrochloric acid (twice) and a saturated brine (twice), and dried over anhydrous sodium sulfate. The desiccant is removed by filtration, and the filtrate is concentrated under reduced pressure. The residue is suspended in ethanol, and the precipitates are collected by filtration.

후처리

  1. temperaturethe mixture is refluxed
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washThe organic layer is washed with 1N hydrochloric acid (twice) and a saturated brine (twice), and
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe desiccant is removed by filtration
  7. concentrationthe filtrate is concentrated under reduced pressure
  8. filtrationthe precipitates are collected by filtration

출처 및 근거

ORD 기록
ord-78e0cf40f386481aa4f06f0069be9b7d
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06048854

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