4-Bromophenol → 1-Bromo-4-[3-(methylsulfanyl)propoxy]benzene

HRID 1877194노트

반응식

HRID 1877194 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[CH3:9][S:10][CH2:11][CH2:12][CH2:13]O.C(P(CCCC)CCCC)CCC.N(C(N1CCCCC1)=O)=NC(N1CCCCC1)=O>O1CCCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:13][CH2:12][CH2:11][S:10][CH3:9])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 78084-BromophenolHCID 104483-(Methylthio)-1-propanolHCID 13831TributylphosphineHCID 730421,1'-(Azodicarbonyl)dipiperidine

생성물 1

HCID 685115371-Bromo-4-[3-(methylsulfanyl)propoxy]benzene수율 89.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-bromophenol (3.4 g) and 3-methylthio-1-propanol (2.6 g) in tetrahydrofuran (20 mL) were added tributylphosphine (7.5 mL) and 1,1′-(azodicarbonyl)dipiperidine (7.6 g), and the mixture was stirred at room temperature for 2 hr. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column (0% ethyl acetate/hexane to 20% ethyl acetate/hexane) to give the title compound (4.6 g, 83%) as a white crystal.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by silica gel column (0% ethyl acetate/hexane to 20% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-708dcdf0154147748cbbed7f3495007c
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309580B2

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