1-Hydroxybenzotriazole → HCID 67067277、化合物

HRID 599592ノート

反応式

HRID 599592 の反応式
C(N(C(C)C)CC)(C)C.C1C=CC2N(O)N=NC=2C=1.[F:20][C:21]1[CH:26]=[CH:25][C:24]([CH:27]([CH2:32][CH2:33][OH:34])[C:28]([NH:30][NH2:31])=[O:29])=[CH:23][CH:22]=1.[CH3:35][O:36][C:37]1[CH:38]=[C:39](/[CH:49]=[CH:50]/[C:51](O)=[O:52])[CH:40]=[CH:41][C:42]=1[N:43]1[CH:47]=[C:46]([CH3:48])[N:45]=[CH:44]1>CN(C=O)C.[Cl-].[Na+].O.C(OCC)(=O)C.C(Cl)CCl>[CH3:35][O:36][C:37]1[CH:38]=[C:39](/[CH:49]=[CH:50]/[C:51]([NH:31][NH:30][C:28](=[O:29])[CH:27]([C:24]2[CH:25]=[CH:26][C:21]([F:20])=[CH:22][CH:23]=2)[CH2:32][CH2:33][OH:34])=[O:52])[CH:40]=[CH:41][C:42]=1[N:43]1[CH:47]=[C:46]([CH3:48])[N:45]=[CH:44]1

参加物

9

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 59528030(E)-3-[3-methoxy-4-(4-methylimidazol-1-yl)phenyl]acrylic acidHCID 67067321HCID 67067321、化合物

生成物 1

HCID 67067277HCID 67067277、化合物収率 100.1%

試薬・触媒・溶媒 4

HCID 111,2-Dichloroethane溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

IPEA (0.17 mL), HOBT (134 mg) and EDC (190 mg) were added to a solution of 2-(4-fluorophenyl)-4-hydroxybutyric acid hydrazide (105 mg) and (E)-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acrylic acid (153 mg) in DMF (3 mL), and the reaction solution was stirred at room temperature for 14 hours. Ethyl acetate and brine were added to the reaction solution, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 224 mg of the title compound. The property value of the compound is as follows.

後処理

  1. customthe organic layer was separated
  2. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-79810835226740b2a425f4b3e48ad9db
出典データセット
uspto-grants-2011_03
特許番号
US07897632B2

反応ノート

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