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

HRID 257683
ノート
印刷プレビュー

反応式

HRID 257683 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 6

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒HCID 21883165Tetrahydrofuran hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c069cc17e4664a2fa4e6d624e4865cd8
出典データセット
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05262556

反応ノート

読み込み中…

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