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

HRID 69568

반응식

HRID 69568 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 866551792',4'-Difluorobiphenyl-4-sulfonic acid수율 40.3%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d4c90947511b46f4b333d6a0cdd8281c
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822507B2

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