반응 #344865

ord-c069cc17e4664a2fa4e6d624e4865cd8

반응 방정식

CCCCCc1ccc(-c2ccc(CCc3cc(F)cc(F)c3)cc2)cc1
1-(4'-pentylbiphenyl-4-yl)-2-(3,5-difluorophenyl)ethane
CC1CN1C(=O)N(C)C
N,N-dimethylpropyleneurea
CCCI
1-iodopropane
CC(C)[N-]C(C)C.[Li+]
lithium diisopropylamide
CC(C)NC(C)C
diisopropylamine
[Li][CH2]CCC
n-butyllithium
CCCCCc1ccc(-c2ccc(CCc3cc(F)c(CCC)c(F)c3)cc2)cc1
1-(4'-pentylbiphenyl-4-yl)-2-(3,5-di-fluoro-4-propylphenyl)ethane

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the phases are separated
  2. 2
    추출the aqueous phase is extracted with 2×50 ml of methylene chloride
  3. 3
    건조Drying over magnesium sulfate, evaporation of the solvent and chromatography
  4. 4
    기타give the pure product

실험 절차

A solution of lithium diisopropylamide (0.02 mol) in THF/hexane, prepared from 0.02 mol of diisopropylamine in 25 ml of THF and 12.5 ml of a 1.6-molar solution of n-butyllithium in hexane, is added dropwise at 25° C. to a mixture of 0.02 mol of 1-(4'-pentylbiphenyl-4-yl)-2-(3,5-difluorophenyl)ethane, 0.02 mol of N,N-dimethylpropyleneurea, 0.02 mol of 1-iodopropane and 25 ml of THF. After stirring at room temperature for 1.5 hours, the reaction mixture is poured into water, the phases are separated, and the aqueous phase is extracted with 2×50 ml of methylene chloride. Drying over magnesium sulfate, evaporation of the solvent and chromatography give the pure product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05262556uspto-grants-1993_11