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Diisopropylamine → 4-[2-(3,5-Difluoro-4-propylphenyl)ethyl]-4'-pentyl-1,1'-biphenyl

HRID 257683
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인쇄 미리보기

반응식

HRID 257683 반응식
C([N-][CH:5]([CH3:7])[CH3:6])(C)C.[Li+].C(NC(C)C)(C)C.C([Li])CCC.[CH2:21]([C:26]1[CH:31]=[CH:30][C:29]([C:32]2[CH:37]=[CH:36][C:35]([CH2:38][CH2:39][C:40]3[CH:45]=[C:44]([F:46])[CH:43]=[C:42]([F:47])[CH:41]=3)=[CH:34][CH:33]=2)=[CH:28][CH:27]=1)[CH2:22][CH2:23][CH2:24][CH3:25].CC1N(C(N(C)C)=O)C1.ICCC>C1COCC1.CCCCCC.C1COCC1.CCCCCC.O>[CH2:21]([C:26]1[CH:31]=[CH:30][C:29]([C:32]2[CH:37]=[CH:36][C:35]([CH2:38][CH2:39][C:40]3[CH:41]=[C:42]([F:47])[C:43]([CH2:7][CH2:5][CH3:6])=[C:44]([F:46])[CH:45]=3)=[CH:34][CH:33]=2)=[CH:28][CH:27]=1)[CH2:22][CH2:23][CH2:24][CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 6

HCID 7912DiisopropylamineHCID 336431-IodopropaneHCID 2724682Lithium diisopropylamideHCID 11007919N,N,2-trimethylaziridine-1-carboxamideHCID 157248231-(4'-Pentylbiphenyl-4-yl)-2-(3,5-difluorophenyl)ethaneHCID 178418339Butyllithium

생성물 1

HCID 19783700
4-[2-(3,5-Difluoro-4-propylphenyl)ethyl]-4'-pentyl-1,1'-biphenyl

시약·촉매·용매 4

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매HCID 21883165Tetrahydrofuran hexane용매

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.

후처리

  1. customthe phases are separated
  2. extractionthe aqueous phase is extracted with 2×50 ml of methylene chloride
  3. dry with materialDrying over magnesium sulfate, evaporation of the solvent and chromatography
  4. customgive the pure product

출처 및 근거

ORD 기록
ord-c069cc17e4664a2fa4e6d624e4865cd8
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05262556

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