tert-Butyl hydroperoxide → 2,3-Difluoro-4-octyloxyphenyl 4-hexyloxybenzoate

HRID 6331

반응식

HRID 6331 반응식
[CH2:1]([O:7][C:8]1[CH:16]=[CH:15][C:11]([C:12]([OH:14])=[O:13])=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].CN(C1C=CC=CN=1)C.[F:26][C:27]1[C:32]([F:33])=[C:31]([O:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])[CH:30]=[CH:29][C:28]=1O.FC(C(F)CCCCC)COC1C=CC=CC=1.C(OOC(C)(C)C)(C)(C)C.[Li].C(OO)(C)(C)C.C([Li])CCC.C1(N=C=NC2CCCCC2)CCCCC1>CCOCC.ClCCl>[CH2:1]([O:7][C:8]1[CH:9]=[CH:10][C:11]([C:12]([O:14][C:28]2[CH:29]=[CH:30][C:31]([O:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])=[C:32]([F:33])[C:27]=2[F:26])=[O:13])=[CH:15][CH:16]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

11

반응물 8

HCID 6410tert-Butyl hydroperoxideHCID 10868DicyclohexylcarbodiimideHCID 218852-DimethylaminopyridineHCID 708344-(Hexyloxy)benzoic acidHCID 147667032,3-Difluoro-4octyloxyphenolHCID 191036322,3-DifluorooctyloxybenzeneHCID 86747250CID 86747250HCID 178418339Butyllithium

생성물 1

HCID 191037182,3-Difluoro-4-octyloxyphenyl 4-hexyloxybenzoate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매2회

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.

후처리

  1. filtrationThe mixture is filtered through silica gel
  2. customthe solvent is evaporated

출처 및 근거

ORD 기록
ord-82e83c02b9134508a72b2b79ba90c519
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05248447

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