Chlorosulfonic acid → 2',4'-Difluorobiphenyl-4-sulfonic acid

HRID 69568

反応式

HRID 69568 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.Cl[S:16]([OH:19])(=[O:18])=[O:17]>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([S:16]([OH:19])(=[O:18])=[O:17])=[CH:11][CH:10]=1

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 1699742,4-Difluoro-1,1'-biphenyl

生成物 1

HCID 866551792',4'-Difluorobiphenyl-4-sulfonic acid収率 40.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

2,4-Difluorobiphenyl (21.2 g, 111 mmol) was dissolved in chloroform (120 mL) and chlorosulfonic acid (12.5 mL, 188 mmol) was added dropwise. The mixture was stirred overnight at room temperature. The reaction mixture was concentrated in vacuo and the residue taken up into EtOAc (100 mL) and washed with water (3×25 mL). The organics were shaken with brine, whereupon a flocculent solid formed. This was filtered and washed with EtOAc and dried to give 2′,4′-difluorobiphenyl-4-sulfonic acid as an off-white solid (12.1 g).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. washwashed with water (3×25 mL)
  3. stirringThe organics were shaken with brine, whereupon a flocculent solid
  4. customformed
  5. filtrationThis was filtered
  6. washwashed with EtOAc
  7. customdried

出典と根拠

ORDレコード
ord-d4c90947511b46f4b333d6a0cdd8281c
出典データセット
uspto-grants-2014_09
特許番号
US08822507B2

関連ノート

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