Potassium Carbonate → 5-Chloropyrazinoic acid
反応式
[Cl:1][C:2]1[N:3]=[CH:4][C:5]([C:8]([O:10]C)=[O:9])=[N:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+]>CO.O>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([C:8]([OH:10])=[O:9])=[N:6][CH:7]=1参加物
5
実験手順
A solution of methyl 5-chloro-2-pyrazinecarboxylate (Bio-Farma; 1.50 g, 8.69 mmol) in a mixture of methanol (16 ml) and water (8 ml) was stirred at room temperature and treated with potassium carbonate (1.201 g, 8.69 mmol). The resulting solution was stirred for 2 hrs and the methanol removed under reduced pressure. The residue was partitioned between ethyl acetate and water (20 ml) and the aqueous layer acidified by addition of 5M hydrochloric acid. Extraction (×2) with ethyl acetate and drying over MgSO4 followed by removal of the solvent under reduced pressure, gave the title compound (1.00 g) as a white solid;
後処理
- stirringThe resulting solution was stirred for 2 hrs
- customthe methanol removed under reduced pressure
- customThe residue was partitioned between ethyl acetate and water (20 ml)
- additionthe aqueous layer acidified by addition of 5M hydrochloric acid
- extractionExtraction (×2) with ethyl acetate
- dry with materialdrying over MgSO4
- customfollowed by removal of the solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-ba30737b57bc4b459ce1bb5842ea681e
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08377941B2
反応ノート
読み込み中…