Phosphorus oxychloride → 3-Chloro-6-methoxypyrazin-2-amine
反応式
[NH2:1][C:2]1[CH:7]=[N+:6]([O-])[CH:5]=[C:4]([O:9][CH3:10])[N:3]=1.P(Cl)(Cl)([Cl:13])=O>>[NH2:1][C:2]1[C:7]([Cl:13])=[N:6][CH:5]=[C:4]([O:9][CH3:10])[N:3]=1参加物
3
実験手順
A suspension of 2-amino-6-methoxypyrazine 4-oxide in freshly distilled phosphorus oxychloride is refluxed for one hour. Thin layer chromatography indicates that the starting material is no longer present. The excess of phosphorus oxychloride is removed in vacuo and the residue is treated with crushed ice. If decomposition is complete the solution is made alkaline with 10% sodium hydroxide and extracted with chloroform. The chloroform extracts are washed with water, dried over sodium sulfate and evaporated to give the product which may be recrystallized from a suitable solvent such as ethanol.
後処理
- temperatureis refluxed for one hour
- customThe excess of phosphorus oxychloride is removed in vacuo
- additionthe residue is treated with crushed ice
- extractionextracted with chloroform
- washThe chloroform extracts are washed with water
- dry with materialdried over sodium sulfate
- customevaporated
- customto give the product which
- custommay be recrystallized from a suitable solvent such as ethanol
出典と根拠
- ORDレコード
- ord-d21f8adf8297470da7103afcdb971758
- 出典データセット
- uspto-grants-1977_08
- 特許番号
- US04042586
反応ノート
読み込み中…