Sodium Hydroxide → 5-(Methoxymethyl)pyridine-2,3-dicarboxylic acid
反応式
[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([C:14]([O:16]C)=[O:15])[C:7]([C:10]([O:12]C)=[O:11])=[N:8][CH:9]=1.[OH-].[Na+]>O>[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([C:14]([OH:16])=[O:15])[C:7]([C:10]([OH:12])=[O:11])=[N:8][CH:9]=1参加物
4
反応条件
- 温度
- 100 °C
実験手順
A mixture of dimethyl 5-(methoxymethyl)-2,3-pyridinedicarboxylate (60.0 g, 0.25 mol) and 50% sodium hydroxide solution (50.0 g, 0.63 mol) in water is heated at 90-110° C. for 2 hours under nitrogen while distilling off methanol and water. The reaction mixture is cooled to 10° C., treated with sulfuric acid to adjust the pH to 2.0 and filtered to obtain a solid. The solid is washed with water and vacuum dried to give the title product as a white solid (44.3 g, mp 161-162° C.).
後処理
- distillationwhile distilling off methanol and water
- temperatureThe reaction mixture is cooled to 10° C.
- additiontreated with sulfuric acid
- filtrationfiltered
- customto obtain a solid
- washThe solid is washed with water and vacuum
- customdried
出典と根拠
- ORDレコード
- ord-2f483b3b67d3498bb722df2b7e573410
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096570B2
反応ノート
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