Water → 4'-Bromo-4-carboxymethylbiphenyl

HRID 1004515

反応式

HRID 1004515 の反応式
[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

参加物

5

反応物 4

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

生成物 1

HCID 13942454'-Bromo-4-carboxymethylbiphenyl

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-78e0cf40f386481aa4f06f0069be9b7d
出典データセット
uspto-grants-2000_04
特許番号
US06048854

関連ノート

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