반응식
[Br:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([Br:11])=[CH:4][N:3]=1.Cl[Sn]Cl>C(O)C>[Br:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([Br:11])=[CH:4][N:3]=1참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
To the solution of 2,5-Dibromo-3-nitro-pyridine (10.30 g, 35.47 mmol) in the 100 ml of ethanol was added SnCl2 (24.0 g, 106.42 mmol) slowly. The reaction mixture was heated at 80° C. for 2 h. After the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure. Water (250 mL) was added, white solid separated out, then, basified the reaction mixture with NaOH Solution. To this added the 250 ml of ethyl acetate. Filtered it and washed the residue with ethyl acetate, layers are separated, dried (Na2SO4), filtered, concentrated to give the desired product (6.20 g, 67.39%).
후처리
- customAfter the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure
- additionWater (250 mL) was added
- customwhite solid separated out
- additionTo this added the 250 ml of ethyl acetate
- filtrationFiltered it
- washwashed the residue with ethyl acetate, layers
- customare separated
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-c271af90fdd74c5d8dee0187082e140a
- 출처 데이터셋
- uspto-grants-2014_10
- 특허 번호
- US08865736B2
연결된 노트
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