Sodium Phosphate, Dibasic → 1-Methyl-5-(methylthio)-1H-pyrazol-3-amine
反応式
[NH2:1][C:2]1[C:6](C#N)=[C:5]([S:9][CH3:10])[N:4]([CH3:11])[N:3]=1.P([O-])([O-])(O)=O.[Na+].[Na+]>[OH-].[Na+]>[NH2:1][C:2]1[CH:6]=[C:5]([S:9][CH3:10])[N:4]([CH3:11])[N:3]=1参加物
4
反応条件
- 温度
- 50 °C
実験手順
5.55 g (33.0 mmol) 3-amino-4-cyano-1-methyl-5-methylmercaptopyrazole heated with 50 ml 32% caustic soda at boiling for 24 hours. The reaction mixture was cooled, made slightly acidic with aqueous sodium hydrogen phosphate, heated for 8 hours at 50° C. and extracted with ethyl acetate. The organic phase was dried over sodium sulfate, concentrated and the residue purified by silica gel chromatography (hexane/ethyl acetate 1:1).
後処理
- temperatureThe reaction mixture was cooled
- extractionextracted with ethyl acetate
- dry with materialThe organic phase was dried over sodium sulfate
- concentrationconcentrated
- customthe residue purified by silica gel chromatography (hexane/ethyl acetate 1:1)
出典と根拠
- ORDレコード
- ord-c1a7f84277e14cdcbba2764d7cd70a90
- 出典データセット
- uspto-grants-1999_02
- 特許番号
- US05869686
反応ノート
読み込み中…