Sodium Chloride → N-tert-Butyl-2-nitroaniline

HRID 2110383ノート

反応式

HRID 2110383 の反応式
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[C:11]([NH2:15])([CH3:14])([CH3:13])[CH3:12].[Cl-].[Na+]>CN(C)C=O>[C:11]([NH:15][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9])([CH3:14])([CH3:13])[CH3:12]

参加物

5

実験手順

To a solution of 1-fluoro-2-nitro-benzene (1 g, 7.1 mmol) in dimethylformamide (15 mL) was added tert-butyl amine (0.82 mL, 7.81 mmol) at room temperature, and the reaction mixture stirred for 12 hours at room temperature under nitrogen. Upon completion, the reaction mixture was poured into a saturated aqueous solution of sodium chloride (50 mL) and extracted with ethyl acetate (50 mL). The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo, and the residue was purified via flash column chromatography (silica, 1% ethyl acetate in hexane) to give tert-butyl-(2-nitrophenyl)-amine as an orange oil. MS (ES) m/z 195.2

後処理

  1. extractionextracted with ethyl acetate (50 mL)
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customthe residue was purified via flash column chromatography (silica, 1% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-203045e470a64bd19e18d29810cf970e
出典データセット
uspto-grants-2009_04
特許番号
US07517899B2

反応ノート

読み込み中…