تفاعل #344865

ord-c069cc17e4664a2fa4e6d624e4865cd8

معادلة التفاعل

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

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe phases are separated
  2. 2
    استخلاصthe aqueous phase is extracted with 2×50 ml of methylene chloride
  3. 3
    تجفيفDrying over magnesium sulfate, evaporation of the solvent and chromatography
  4. 4
    أخرىgive the pure product

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05262556uspto-grants-1993_11