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

HRID 31426
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HRID 31426 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 11
1,2-Dichloroethane
용매
HCID 6228Dimethylformamide용매

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온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-47dc77586e68474399b3b016fddb9e26
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07425555B2

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