Chloroform → 2,4-Difluoro-5-methylbenzenesulfonyl chloride

HRID 1402071

반응식

HRID 1402071 반응식
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[CH3:14].C(Cl)(Cl)Cl>>[F:13][C:11]1[CH:12]=[C:7]([F:6])[C:8]([CH3:14])=[CH:9][C:10]=1[S:2]([Cl:1])(=[O:5])=[O:3]

참가 물질

4

반응물 3

HCID 6212ChloroformHCID 24638Chlorosulfonic acid2회HCID 679832,4-Difluoro-1-methylbenzene

생성물 1

HCID 594365302,4-Difluoro-5-methylbenzenesulfonyl chloride수율 75.1%

실험 절차

Chlorosulfonic acid (5.2 mL, 0.078 mol) was added dropwise to a solution of 2,4-difluorotoluene (4.00 g, 0.0312 mol) in chloroform (75 mL, 0.94 mol). The reaction was stirred 2 hours. Additional chlorosulfonic acid (3.1 mL, 0.047 mol) was added and stirring was continued for 18 hours. The reaction was evaporated to an oil and poured onto ice. The mixture was extracted two times with ethyl ether. The combined organic phase was dried over magnesium sulfate and treated with activated carbon. The mixture was filtered through diatomaceous earth and the filtrate was evaporated to give 5.31 g of light brown oil.

후처리

  1. stirringstirring
  2. waitwas continued for 18 hours
  3. customThe reaction was evaporated to an oil
  4. additionpoured onto ice
  5. extractionThe mixture was extracted two times with ethyl ether
  6. dry with materialThe combined organic phase was dried over magnesium sulfate
  7. additiontreated with activated carbon
  8. filtrationThe mixture was filtered through diatomaceous earth
  9. customthe filtrate was evaporated

출처 및 근거

ORD 기록
ord-c566f74ba0cc4c9e9fa41db9f2e572a0
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08907101B2

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