Water → 3-Amino-2-bromo-6-chloropyridine-4-carboxylic acid
反応式
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]参加物
6
実験手順
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
後処理
- 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
出典と根拠
- ORDレコード
- ord-eba12bab327142c098fcb7e4972ccede
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08247431B2
反応ノート
読み込み中…