Formic Acid → 1-(2-Bromo-4-fluorophenyl)-2,2,2-trifluoroethan-1-amine
反応式
[N:1]([CH:4]([C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=1[Br:16])[C:5]([F:8])([F:7])[F:6])=[N+]=[N-].C(O)=O.NN>[Ni].C(O)C>[Br:16][C:10]1[CH:11]=[C:12]([F:15])[CH:13]=[CH:14][C:9]=1[CH:4]([NH2:1])[C:5]([F:6])([F:7])[F:8]参加物
6
実験手順
Add Raney Nickel (1.58 g, 26.8 mmol) to a solution of 1-(1-azido-2,2,2-trifluoro-ethyl)-2-bromo-4-fluoro-benzene (0.8 g, 2.68 mmol), formic acid (1.24 g, 26.8 mmol), and hydrazine (0.86 g, 26.8 mmol) in 10 mL of ethanol. Stir the mixture at RT for 1 h and filter off the excess Nickel. Dilute the mother liquor with water and extract with chloroform. Dry the organic layer over sodium sulfate and concentrate to give the title compound as a brown oil (0.73 g, 100%). MS (ES) m/z 272/274 [M+1]+.
後処理
- filtrationfilter off the excess Nickel
- additionDilute the mother liquor with water
- extractionextract with chloroform
- dry with materialDry the organic layer over sodium sulfate
- concentrationconcentrate
出典と根拠
- ORDレコード
- ord-7aad3f7a12704229ae59c0330403a36c
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063035B2
反応ノート
読み込み中…