1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 16222146、化合物

HRID 1717428ノート

反応式

HRID 1717428 の反応式
[CH:1](/[C:4]1[N:8]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([NH:17][CH2:18][C:19]([F:22])([F:21])[F:20])=[O:16])=[CH:11][CH:10]=2)[N:7]=[N:6][C:5]=1[C:23](O)=[O:24])=[CH:2]\[CH3:3].[CH:26]1([NH2:29])[CH2:28][CH2:27]1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C>CN(C=O)C.C(OCC)(=O)C.O.C(N(CC)CC)C>[CH:26]1([NH:29][C:23]([C:5]2[N:6]=[N:7][N:8]([C:9]3[CH:14]=[CH:13][C:12]([C:15]([NH:17][CH2:18][C:19]([F:20])([F:21])[F:22])=[O:16])=[CH:11][CH:10]=3)[C:4]=2/[CH:1]=[CH:2]/[CH3:3])=[O:24])[CH2:28][CH2:27]1

参加物

9

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 69828CyclopropylamineHCID 757711-HydroxybenzotriazoleHCID 68515283HCID 68515283、化合物

生成物 1

HCID 16222146HCID 16222146、化合物収率 52%

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 5-[(1E)-prop-1-en-1-yl]-1-(4-{[(2,2,2-trifluoroethyl)amino]carbonyl}phenyl)-1H-1,2,3-triazole-4-carboxylic acid (1.96 g) obtained in Example 1215a) in DMF (22 ml) were successively added cyclopropylamine (0.46 ml), triethylamine (0.92 ml), HOBt (1.01 g) and WSC (1.27 g), and the reaction mixture was stirred at room temperature for 2.5 hr. Water and ethyl acetate were added to the reaction mixture and the organic layer was separated. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (ethyl acetate/hexane=1/1 to ethyl acetate) and recrystallized from ethyl acetate-diisopropyl ether to give the title compound as a white powder (1.13 g, 52%).

後処理

  1. customthe organic layer was separated
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column (ethyl acetate/hexane=1/1 to ethyl acetate)
  5. customrecrystallized from ethyl acetate-diisopropyl ether

出典と根拠

ORDレコード
ord-d8153be25fdb4657a77f0ee94e6ac9a4
出典データセット
uspto-grants-2010_09
特許番号
US07803822B2

反応ノート

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