Trifluoroacetic acid → 4-(4-Amino-phenoxy)-N-(4-bromo-phenyl)-3-nitro-benzamide

HRID 605136

反応式

HRID 605136 の反応式
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21](=[O:30])[NH:22][C:23]3[CH:28]=[CH:27][C:26]([Br:29])=[CH:25][CH:24]=3)=[CH:17][C:16]=2[N+:31]([O-:33])=[O:32])=[CH:10][CH:9]=1)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[NH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([NH:22][C:23]3[CH:28]=[CH:27][C:26]([Br:29])=[CH:25][CH:24]=3)=[O:30])=[CH:17][C:16]=2[N+:31]([O-:33])=[O:32])=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67040702{4-[4-(4-Bromo-phenylcarbamoyl)-2-nitro-phenoxy]phenyl}-carbamic acid tert-butyl ester

生成物 1

HCID 670405064-(4-Amino-phenoxy)-N-(4-bromo-phenyl)-3-nitro-benzamide収率 97.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of the product of Example 10B (250 mg, 0.4732 mmol) in methylene chloride (5 mL) was treated with trifluoroacetic acid (5 mL) at room temperature for 30 minutes. The solvents were removed by rotary evaporation under vacuum, and the residue taken up in ethyl acetate (100 mL) and washed with saturated aqueous sodium hydrogen carbonate (2×50 mL), water (50 mL), and brine (50 mL). The organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated under vacuum to provide the title compound as a light orange solid (197 mg, 97%).

後処理

  1. customThe solvents were removed by rotary evaporation under vacuum
  2. washwashed with saturated aqueous sodium hydrogen carbonate (2×50 mL), water (50 mL), and brine (50 mL)
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-ab2b9c3289ac4e2fa2c278a73a4f920c
出典データセット
uspto-grants-2011_03
特許番号
US07910595B2

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