Chlorosulfonic acid → 4-((S)-2-Fluoro-1-methyl-ethyl)-benzenesulfonyl chloride

HRID 390297

반응식

HRID 390297 반응식
[F:1][CH2:2][C@H:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH3:4].[Cl:11][S:12](O)(=[O:14])=[O:13]>ClCCl>[F:1][CH2:2][C@H:3]([C:5]1[CH:10]=[CH:9][C:8]([S:12]([Cl:11])(=[O:14])=[O:13])=[CH:7][CH:6]=1)[CH3:4]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 53628601((S)-2-Fluoro-1-methyl-ethyl)-benzene

생성물 1

HCID 536286004-((S)-2-Fluoro-1-methyl-ethyl)-benzenesulfonyl chloride수율 25%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
30 °C

실험 절차

3.5 g of ((S)-2-fluoro-1-methyl-ethyl)-benzene (25.32 mmol) were dissolved in 80 ml of dichloromethane. At 0-5° C., 11.81 g of chlorosulfonic acid (101.31 mmol), dissolved in 20 ml of dichloromethane, were added dropwise. The reaction mixture was stirred for 30 min at room temperature and 2 h at 30° C. The solvent was evaporated. 150 ml of diethyl ether were added to the residue, washed once with 150 ml of water, and the organic layer was dried over magnesium sulfate, filtered, and the solvent was evaporated under reduced pressure. The crude product was purified via silica gel chromatography with n-heptane-dichloromethane (6:4) as eluent to give 1.5 g of the title compound.

후처리

  1. additionwere added dropwise
  2. customThe solvent was evaporated
  3. addition150 ml of diethyl ether were added to the residue
  4. washwashed once with 150 ml of water
  5. dry with materialthe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent was evaporated under reduced pressure
  8. customThe crude product was purified via silica gel chromatography with n-heptane-dichloromethane (6:4) as eluent

출처 및 근거

ORD 기록
ord-9f9e70e39417427899bd2496818375b6
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08383641B2

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