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Methoxyacetic Acid → HCID 68516671、化合物

HRID 1717238
ノート
印刷プレビュー

反応式

HRID 1717238 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12]([CH2:13][CH2:14][CH3:15])=[C:11]([C:16]([NH:18][CH:19]3[CH2:21][CH2:20]3)=[O:17])[N:10]=[N:9]2)=[CH:4][CH:3]=1.[CH3:22][O:23][CH2:24][C:25](O)=[O:26].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C>C(#N)C.C(N(CC)CC)C>[CH:19]1([NH:18][C:16]([C:11]2[N:10]=[N:9][N:8]([C:5]3[CH:6]=[CH:7][C:2]([NH:1][C:25](=[O:26])[CH2:24][O:23][CH3:22])=[CH:3][CH:4]=3)[C:12]=2[CH2:13][CH2:14][CH3:15])=[O:17])[CH2:20][CH2:21]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 12251Methoxyacetic AcidHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 685175481-(4-aminophenyl)-N-cyclopropyl-5-propyl-1H-1,2,3-triazole-4-carboxamide

生成物 1

HCID 68516671HCID 68516671、化合物

試薬・触媒・溶媒 2

HCID 6342
Acetonitrile
溶媒
HCID 8471Triethylamine溶媒

実験手順

To a solution of 1-(4-aminophenyl)-N-cyclopropyl-5-propyl-1H-1,2,3-triazole-4-carboxamide (0.29 g) obtained in Example 1d) in acetonitrile (10 ml) were successively added methoxyacetic acid (0.08 ml), triethylamine (0.17 ml), HOBt (0.18 g) and WSC (0.23 g), and the mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate and washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous magnesium 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 the obtained product was recrystallized from ethanol-water to give the title compound as colorless needle crystals (0.16 g, 44%).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with saturated aqueous sodium hydrogen carbonate solution
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column (ethyl acetate/hexane=1/1 to ethyl acetate)
  7. customthe obtained product was recrystallized from ethanol-water

出典と根拠

ORDレコード
ord-385df3ee0ba64164b4e9df0e2fc80d7c
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803822B2

反応ノート

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