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HCID 86623751, 화합물 → HCID 66998716, 화합물

HRID 1161816
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HRID 1161816 반응식
[C:1]([O:5][C:6]([C:8]1[C:13]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([Br:21])=[CH:17][C:16]=2[F:22])=[CH:12][C:11]([N:24]=[N+]=[N-])([Cl:23])[NH:10][N:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>[Zn].C(OCC)(=O)C>[C:1]([O:5][C:6]([C:8]1[C:13]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([Br:21])=[CH:17][C:16]=2[F:22])=[CH:12][C:11]([NH2:24])([Cl:23])[NH:10][N:9]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

4

반응물 1

HCID 86623751HCID 86623751, 화합물

생성물 1

HCID 66998716HCID 66998716, 화합물

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 8857Ethyl Acetate용매

실험 절차

To the stirred solution of 6-azido-4-(4-bromo-2-fluoro-phenylamino)-6-chloro-pyridazine-3-carboxylic acid tert-butyl ester (122 mg, 0.30 mmol) in 5 ml of mixed solvents (3:1 v/v, dichloromethane/acetic acid) is added zinc powder (98 mg, 1.5 mmol) at room temperature. After three hours, the reaction mixture is poured into ethyl acetate (50 μl). The organic layer is washed with water, saturated NaHCO3 (30 ml×3) and saturated NaCl (30 ml×3). The organic layer is dried over Na2SO4, and concentrated. The residue is purified by flash column chromatography to provide the desired product.

후처리

  1. washThe organic layer is washed with water, saturated NaHCO3 (30 ml×3) and saturated NaCl (30 ml×3)
  2. dry with materialThe organic layer is dried over Na2SO4
  3. concentrationconcentrated
  4. customThe residue is purified by flash column chromatography

출처 및 근거

ORD 기록
ord-f1a656354b8f4cbb93484056a715f285
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820664B2

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