Water → 4-Bromo-2-chloro-1-(ethylsulfanyl)benzene

HRID 70579

반응식

HRID 70579 반응식
[CH2:1]([S-:3])[CH3:2].[Na+].[Br:5][C:6]1[CH:11]=[CH:10][C:9](F)=[C:8]([Cl:13])[CH:7]=1.O>CN(C)C=O>[Br:5][C:6]1[CH:11]=[CH:10][C:9]([S:3][CH2:1][CH3:2])=[C:8]([Cl:13])[CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 35430654-Bromo-2-chloro-1-fluorobenzeneHCID 4459711Sodium ethanethiolate

생성물 1

HCID 584523264-Bromo-2-chloro-1-(ethylsulfanyl)benzene수율 80.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
65 °C

실험 절차

Sodium ethanethiolate (2.0 g) was added to a solution of 4-bromo-2-chloro-1-fluorobenzene (5.0 g) in N,N-dimethylformamide (20 mL), and the mixture was stirred at 65° C. for two hours. The reaction solution was poured into water, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:1→0:100) to give the title compound as a colorless oil (4.8 g).

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was then evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:1→0:100)

출처 및 근거

ORD 기록
ord-a2e05521131d48fa887d2bc0d813faf0
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822503B2

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