Hydrochloric Acid → 4-Hydroxy-1-Methyl-1h-pyridin-2-one
反応式
[OH:1][C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[CH:4][N:3]=1.S(OC)(O[CH3:13])(=O)=O.Cl>[OH-].[Na+]>[OH:8][C:6]1[CH:5]=[CH:4][N:3]([CH3:13])[C:2](=[O:1])[CH:7]=1参加物
5
実験手順
2,4-Dihydroxypyridine (3.0 g) was dissolved in 2N aqueous sodium hydroxide solution (30 ml) and dimethyl sulphate (3.7 g) was added dropwise over 90 minutes. The mixture was stirred at room temperature overnight, acidified with concentrated hydrochloric acid, the solvent removed under reduced pressure, the residue stirred in 5% methanol/dichloromethane and filtered. The filtrate was evaporated and the crude product was chromatographed on silica using 7:93 methanol: dichloromethane as the eluent to yield 1,2-dihydro-4-hydroxy-1-methyl-2-oxopyridine (0.77 g) as a yellow solid. m.p. 165-169° C. Found: C,57.28; H,5.47; N,10.89. C6H7NO2 requires C,57.59; H,5.64; N,11.19%.
後処理
- customthe solvent removed under reduced pressure
- stirringthe residue stirred in 5% methanol/dichloromethane
- filtrationfiltered
- customThe filtrate was evaporated
- customthe crude product was chromatographed on silica using 7:93 methanol
出典と根拠
- ORDレコード
- ord-54e4f9f6404a445cae9caaa153ae5acd
- 出典データセット
- uspto-grants-1999_06
- 特許番号
- US05912244
反応ノート
読み込み中…