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Ethyl Acetate → HCID 90308710、化合物

HRID 2283692
ノート
印刷プレビュー

反応式

HRID 2283692 の反応式
C(OCC)(=O)C.[CH3:7][N:8]1[CH:16]=[C:15]2[C:10]([C:11]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:12][C:13]([N+:17]([O-])=O)=[CH:14]2)=[N:9]1>[Pd].C1COCC1>[CH3:7][N:8]1[CH:16]=[C:15]2[C:10]([C:11]([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)=[CH:12][C:13]([NH2:17])=[CH:14]2)=[N:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8857Ethyl AcetateHCID 90308830HCID 90308830、化合物

生成物 1

HCID 90308710HCID 90308710、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl acetate (5 mL) and THF (2 mL) were added to 2-methyl-5-nitro-7-phenyl-2H-indazole obtained in the above-described Step 2 (260 mg). Thereafter, 10% palladium on carbon (300 mg) was added under nitrogen atmosphere, and the reaction solution was stirred under hydrogen atmosphere at room temperature overnight. The insolubles were filtrated, and then the solvent was evaporated under vacuum. Subsequently, the resultant residue was purified by column chromatography on basic silica gel (developing solvent:hexane/ethyl acetate) to obtain 2-methyl-7-phenyl-2H-indazol-5-amine as brown amorphous.

後処理

  1. customobtained in the above-described Step 2 (260 mg)
  2. filtrationThe insolubles were filtrated
  3. customthe solvent was evaporated under vacuum
  4. customSubsequently, the resultant residue was purified by column chromatography on basic silica gel (developing solvent:hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-c4cb943ba6dc436da8e776c23f5515e3
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09145414B2

反応ノート

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