Chlorosulfonic acid → 3-Bromo-4-(trifluoromethoxy)benzenesulfonyl chloride

HRID 450715노트

반응식

HRID 450715 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][C:9]([F:12])([F:11])[F:10].[Cl:13][S:14](O)(=[O:16])=[O:15]>ClCCl.CCCCCCC.ClCCl>[Br:1][C:2]1[CH:7]=[C:6]([S:14]([Cl:13])(=[O:16])=[O:15])[CH:5]=[CH:4][C:3]=1[O:8][C:9]([F:11])([F:10])[F:12]

참가 물질

5

반응물 2

HCID 24638Chlorosulfonic acidHCID 27772661-Bromo-2-(trifluoromethoxy)benzene

생성물 1

HCID 509980203-Bromo-4-(trifluoromethoxy)benzenesulfonyl chloride수율 77.7%

시약·촉매·용매 2

HCID 6344Dichloromethane용매3회HCID 21907733Dichloromethane heptane용매

실험 절차

2.0 g of 1-bromo-2-(trifluoro-methoxy)benzene (8.3 mmol) were dissolved in 30 ml of dichloromethane. At 0-5° C., 1.06 g of chlorosulfonic acid (9.13 mmol), dissolved in 3 ml of dichloromethane, were added dropwise. The reaction mixture was stirred for 30 min at room temperature. Additional 5.5 equivalents of chlorosulfonic in dichloromethane were added to drive the reaction to completion. Standard work-up was followed and silica gel chromatography with n-heptane-dichloromethane (6:4) as eluent gave 2.19 g of the title compound.

후처리

  1. additionwere added dropwise
  2. customthe reaction to completion

출처 및 근거

ORD 기록
ord-054f0d9409e64f83985fa23ec603e13e
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486984B2

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