Methanol → Methyl pyrazinoate
反応式
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]([OH:9])=[O:8].OS(O)(=O)=O.[CH3:15]O>>[CH3:15][O:8][C:7]([C:2]1[CH:3]=[N:4][CH:5]=[CH:6][N:1]=1)=[O:9]参加物
4
実験手順
A solution of 2-pyrazinecarboxylic acid (2.00 g, 16.1 mmol) and H2SO4 (catalytic) in MeOH (50 mL) was heated at reflux for 45 minutes, then concentrated in vacuo. The residue was partitioned between EtOAc (40 mL) and saturated NaHCO3(aq) (20 mL). The organic phase was washed with saturated NaHCO3(aq) (20 mL) and brine (10 mL), then dried (MgSO4) and concentrated in vacuo to give colourless crystals (1.32 g, 59%). 1H NMR (CDCl3) □ 4.04 (s, 3H), 8.72 (dd, 11H, J=2.4, 1.2 Hz), 8.77 (d, 1H, J=2.4 Hz), 9.32 (d, 1H, J=1.2 Hz).
後処理
- temperatureat reflux for 45 minutes
- concentrationconcentrated in vacuo
- customThe residue was partitioned between EtOAc (40 mL) and saturated NaHCO3(aq) (20 mL)
- washThe organic phase was washed with saturated NaHCO3(aq) (20 mL) and brine (10 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-1245e15db51147829497f5c1ab0ba500
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07084155B2
反応ノート
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