Borane;tetrahydrofuran → (4-Chloro-3-fluoro-5-nitrophenyl)methanamine
반응식
B.C1COCC1.[Cl:7][C:8]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][C:11]([C:12]#[N:13])=[CH:10][C:9]=1[F:19]>C1COCC1>[Cl:7][C:8]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][C:11]([CH2:12][NH2:13])=[CH:10][C:9]=1[F:19]참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
A solution of BH3/THF (7.5 mL; 7.5 mmol) was added dropwise to a solution of 4-chloro-3-fluoro-5-nitrobenzonitrile (750 mg; 3.74 mmol) in THF (5 mL) at 0° C. The mixture was stirred at 0° C. for 3 h, it was acidified to pH ˜1 and stirred at rt for 1 h and then basicified to pH ˜8 and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was dissolved in Et2O and precipitated with PE to give the sub-title compound.
후처리
- stirringstirred at rt for 1 h
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- dissolutionThe residue was dissolved in Et2O
- customprecipitated with PE
출처 및 근거
- ORD 기록
- ord-698ba325855e41bfa5c2f49f178222bc
- 출처 데이터셋
- uspto-grants-2013_06
- 특허 번호
- US08466186B2
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