반응 #6427

ord-82e83c02b9134508a72b2b79ba90c519

반응 방정식

CC(C)(C)OO
t-butyl hydroperoxide
[Li][CH2]CCC
butyllithium
C(=NC1CCCCC1)=NC1CCCCC1
dicyclohexylcarbodiimide
CCCCCCOc1ccc(C(=O)O)cc1
4-hexyloxybenzoic acid
CN(C)c1ccccn1
dimethylaminopyridine
CCCCCCCCOc1ccc(O)c(F)c1F
2,3-difluoro-4octyloxyphenol
CCCCCC(F)C(F)COc1ccccc1
2,3-difluorooctyloxybenzene
CC(C)(C)OOC(C)(C)C.[Li]
lithium t-butylperoxide
CCCCCCCCOc1ccc(OC(=O)c2ccc(OCCCCCC)cc2)c(F)c1F
2,3-difluoro-4-octyloxyphenyl 4-hexyloxybenzoate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture is filtered through silica gel
  2. 2
    기타the solvent is evaporated

실험 절차

0.1 mol of 4-hexyloxybenzoic acid, 0.01 mol of dimethylaminopyridine and 0.1 mol of 2,3-difluoro-4octyloxyphenol (preparable from 2,3-difluorooctyloxybenzene by lithiation at -70° to -80° and dropwise addition of a solution of lithium t-butylperoxide in ether prepared from 0.12 mol of t-butyl hydroperoxide and 0.12 mol of butyllithium) are introduced into 150 ml of dichloromethane, a solution of 0.1 mol of dicyclohexylcarbodiimide in 30 ml of dichloromethane is added dropwise with stirring at 10o, and the mixture is subsequently stirred at room temperature for 15 hours. The mixture is filtered through silica gel, the solvent is evaporated, and 2,3-difluoro-4-octyloxyphenyl 4-hexyloxybenzoate is obtained as the residue.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05248447uspto-grants-1993_09