Methanol → Methyl 3-methylpyrazine-2-carboxylate
反応式
[CH3:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1.[CH3:11]O>S(=O)(=O)(O)O>[CH3:1][C:2]1[C:3]([C:8]([O:10][CH3:11])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1参加物
4
実験手順
A solution of 3-methylpyrazine-2-carboxylic acid (10 g, 72.4 mmol) in 80 mL methanol and sulfuric acid, 95% (5 ml, 90 mmol) was heated to 60° C. for 4 h. The solution was concentrated to remove MeOH, the residue was dissolved in 50 mL of water and neutralized with 10% aq Na2CO3 solution to pH 12. The resulting solution was extracted with ethyl acetate. The combined organics were dried and concentrated to give crude methyl 3-methylpyrazine-2-carboxylate (9.1 g, 83% yield) which was used for next step without further purification.
後処理
- concentrationThe solution was concentrated
- customto remove MeOH
- dissolutionthe residue was dissolved in 50 mL of water and neutralized with 10% aq Na2CO3 solution to pH 12
- extractionThe resulting solution was extracted with ethyl acetate
- customThe combined organics were dried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-133c193d616d4564a7551541c0a115c3
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09309263B2
反応ノート
読み込み中…