Formic Acid → 1-(2-Bromo-4-fluorophenyl)-2,2,2-trifluoroethan-1-amine
반응식
[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]참가 물질
6
실험 절차
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]+.
후처리
- filtrationfilter off the excess Nickel
- additionDilute the mother liquor with water
- extractionextract with chloroform
- dry with materialDry the organic layer over sodium sulfate
- concentrationconcentrate
출처 및 근거
- ORD 기록
- ord-7aad3f7a12704229ae59c0330403a36c
- 출처 데이터셋
- uspto-grants-2011_11
- 특허 번호
- US08063035B2
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