Sodium → methyl 5-amino-1-methyl-1H-pyrazole-3-carboxylate
反応式
[Na].[NH2:2][C:3]1[N:7]([CH3:8])[N:6]=[C:5]([C:9]([O:11][CH2:12]C)=[O:10])[CH:4]=1>CO>[NH2:2][C:3]1[N:7]([CH3:8])[N:6]=[C:5]([C:9]([O:11][CH3:12])=[O:10])[CH:4]=1参加物
4
実験手順
To a solution of 48 mg (2.1 mmol) of sodium in 40 ml of methanol is added 2.0 mg (11.8 mmol) of 5-amino-3-ethoxycarbonyl-1-methylpyrazole, and the mixture is refluxed over night, and distilled under reduced pressure. To the resulting residue are added a small amount of water and sodium chloride, and the mixture is extracted 6 times with chloroform. The extract is dried with magnesium sulfate, chromatographed on a column of silica gel and eluted with ethyl acetate to give 1.37 g (74.1% yield) of the objective compound.
後処理
- temperaturethe mixture is refluxed over night
- distillationdistilled under reduced pressure
- additionTo the resulting residue are added a small amount of water and sodium chloride
- extractionthe mixture is extracted 6 times with chloroform
- dry with materialThe extract is dried with magnesium sulfate
- customchromatographed on a column of silica gel
- washeluted with ethyl acetate
出典と根拠
- ORDレコード
- ord-2acea9e5ebbe4025b45c98ee01e9c12d
- 出典データセット
- uspto-grants-1989_10
- 特許番号
- US04873334
反応ノート
読み込み中…