(1,1'-Biphenyl)-4-sulfonic acid → (1,1'-Biphenyl)-4-sulphonyl chloride

HRID 128714

反応式

HRID 128714 の反応式
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][C:4]([S:7](O)(=[O:9])=[O:8])=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:19])=O>>[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][C:4]([S:7]([Cl:19])(=[O:9])=[O:8])=[CH:3][CH:2]=1

参加物

3

反応物 2

HCID 16673(1,1'-Biphenyl)-4-sulfonic acidHCID 24813Phosphorus oxychloride

生成物 1

HCID 74192(1,1'-Biphenyl)-4-sulphonyl chloride

実験手順

4-Biphenylsulfonic acid (3.0 g, 12.8 mmol) was heated at 70° C. with phosphorus oxychloride (1.30 ml, 14.0 mol) for 2 h. Excess phosphorus oxychloride was removed under reduced pressure. The residue was decomposed with ice water and extracted with ethyl acetate. The extract was washed with 5% sodium bicarbonate solution, dried over anhydrous magnesium sulfate and concentrated to yield 2.9 crude 4-biphenylsulfonyl chloride.

後処理

  1. customExcess phosphorus oxychloride was removed under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with 5% sodium bicarbonate solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-9ed9726190d54b7482c53610f4a193a7
出典データセット
uspto-grants-1995_11
特許番号
US05464853

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