Water → 3-Amino-2-bromo-6-chloropyridine-4-carboxylic acid
반응식
C[O:2][C:3](=[O:13])[C:4]1[CH:9]=[C:8]([Cl:10])[N:7]=[C:6]([Br:11])[C:5]=1[NH2:12].[OH-].[Na+].C(OCC)C.O>CO>[NH2:12][C:5]1[C:6]([Br:11])=[N:7][C:8]([Cl:10])=[CH:9][C:4]=1[C:3]([OH:13])=[O:2]참가 물질
6
실험 절차
3-Amino-2-bromo-6-chloroisonicotinic acid methyl ester (260 mg) (example 3, step 5) was dissolved in methanol (2 mL), 2N aqueous sodium hydroxide solution (2 mL) was added and the reaction mixture was stirred for 2 hours at reflux. After cooling to room temperature, diethyl ether and water were added and the layers were separated. The aqueous layer was washed with diethyl ether and acidified by addition of 2N hydrochloric acid. The formed precipitate was extracted with MTB-ether (3×), the combined organic layer was washed with brine, dried over MgSO4 and concentrated in vacuum to afford 246 mg of
후처리
- temperatureat reflux
- customthe layers were separated
- washThe aqueous layer was washed with diethyl ether
- additionacidified by addition of 2N hydrochloric acid
- extractionThe formed precipitate was extracted with MTB-ether (3×)
- washthe combined organic layer was washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuum
- customto afford 246 mg of
출처 및 근거
- ORD 기록
- ord-eba12bab327142c098fcb7e4972ccede
- 출처 데이터셋
- uspto-grants-2012_08
- 특허 번호
- US08247431B2
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