4-Iodobenzoic acid → 1h-Pyrrole-2-carboxylic acid, 1-methyl-2-(4-iodobenzoyl)hydrazide

HRID 31426

反応式

HRID 31426 の反応式
[CH3:1][N:2]([C:4]([C:6]1[NH:7][CH:8]=[CH:9][CH:10]=1)=[O:5])[NH2:3].C1C=CC2N(O)N=NC=2C=1.[I:21][C:22]1[CH:30]=[CH:29][C:25]([C:26](O)=[O:27])=[CH:24][CH:23]=1.CCN(C(C)C)C(C)C>CN(C=O)C.C(Cl)CCl>[CH3:1][N:2]([C:4]([C:6]1[NH:7][CH:8]=[CH:9][CH:10]=1)=[O:5])[NH:3][C:26](=[O:27])[C:25]1[CH:29]=[CH:30][C:22]([I:21])=[CH:23][CH:24]=1

参加物

7

反応物 4

HCID 120854-Iodobenzoic acidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 701149601H-Pyrrole-2-carboxylic acid, 1-methyl-hydrazide

生成物 1

HCID 693564031h-Pyrrole-2-carboxylic acid, 1-methyl-2-(4-iodobenzoyl)hydrazide

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

1H-Pyrrole-2-carboxylic acid, 1-methyl-hydrazide (139 mg), EDC (230 mg), HOBt (162 mg), 4-iodobenzoic acid (248 mg) and DIPEA (0.21 ml) were mixed in DMF (3 ml). The reaction was heated at 40° C. for 6 hours, the DMF was evaporated under vacuum and the residue applied to a bond-elut (silica) and eluted with an ethyl acetate/cyclohexane gradient to give, after evaporation of the solvent, 1H-pyrrole-2-carboxylic acid, 1-methyl-2-(4-iodobenzoyl)hydrazide.

後処理

  1. customthe DMF was evaporated under vacuum
  2. washeluted with an ethyl acetate/cyclohexane gradient
  3. customto give
  4. customafter evaporation of the solvent, 1H-pyrrole-2-carboxylic acid, 1-methyl-2-(4-iodobenzoyl)hydrazide

出典と根拠

ORDレコード
ord-47dc77586e68474399b3b016fddb9e26
出典データセット
uspto-grants-2008_09
特許番号
US07425555B2

関連ノート

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