Methanol → HCID 67248245、化合物
反応式
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([C:10]=1[CH3:11])[C:7]([OH:9])=[O:8].OS(O)(=O)=O.[CH3:17]O>>[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([C:10]=1[CH3:11])[C:7]([O:9][CH3:17])=[O:8]参加物
4
反応条件
- 温度
- 70 °C
実験手順
To a stirred solution of 5-amino-4-methylnicotinic acid (5.0 g, 32 mmol) in methanol (75 mL), was added conc. H2SO4 (5 mL) slowly at room temperature. The mixture was stirred at 70° C. for 12 h. On completion, the solvent was removed under reduced pressure and the residue was neutralized with saturated NaHCO3 solution. Extraction was carried out using EtOAc; the combined organic layers were washed with water, brine and dried over anhydrous Na2SO4 and concentrated under reduced pressure to give the title compound (4.1 g, 75%) which used without further purification.
後処理
- customOn completion, the solvent was removed under reduced pressure
- extractionExtraction
- washthe combined organic layers were washed with water, brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-5f3f42014dcc4d8ca5894ca41a8cd248
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09376422B2
反応ノート
読み込み中…