Bromine → Methyl 2-amino-5-bromonicotinate
반응식
[Br:1]Br.[NH2:3][C:4]1[N:13]=[CH:12][CH:11]=[CH:10][C:5]=1[C:6]([O:8][CH3:9])=[O:7]>CC(O)=O>[NH2:3][C:4]1[N:13]=[CH:12][C:11]([Br:1])=[CH:10][C:5]=1[C:6]([O:8][CH3:9])=[O:7]참가 물질
4
실험 절차
Bromine (0.7 mL, 14 mmole) was added dropwise to a stirred solution of methyl 2-aminonicotinate (2.0 g, 13 mmole) in HOAc (50 mL). A suspension formed within 30 min. The reaction was allowed to stir at room temperature for 2 h, then was concentrated under vacuum. The residue was triturated with 1.0 N Na2CO3 (50 mL) and the solid was collected by suction filtration. The solid was washed with H2O (50 mL) and dried under vacuum to give the title compound (2.95 g, 98%) as a pale yellow solid: 1H NMR (400 MHz, CDCl3) δ 8.24 (d, J=2.5 Hz, 1 H), 8.23 (d, J=2.5 Hz, 1 H), 6.40 (br s, 2 H), 3.90 (s, 3 H).
후처리
- customA suspension formed within 30 min
- concentrationwas concentrated under vacuum
- customThe residue was triturated with 1.0 N Na2CO3 (50 mL)
- filtrationthe solid was collected by suction filtration
- washThe solid was washed with H2O (50 mL)
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-6b785971e87942358a742a706360fd1c
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07741339B2
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