Hydrochloric Acid → 2-Chloro-4-methoxy-6-methylpyrimidine
反応式
N[C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([O:9][CH3:10])[N:3]=1.N([O-])=O.[Na+].[OH-].[Na+].[ClH:17]>O>[Cl:17][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([O:9][CH3:10])[N:3]=1参加物
6
実験手順
A solution of 25.4 g of 2amino-4-methyl-6-methoxypyrimidine in 150 ml concentrated hydrochloric acid was cooled to ca. 0° C. and treated with a solution of 25.3 g of sodium nitrite in 50 ml water, added over a period of 30-40 minutes. The thick orange reaction mixture was stirred at room temperature for 4-5 hours and then adjusted to pH 10 by addition of 12.5N sodium hydroxide solution. The precipitate was filtered and extracted thoroughly with approximately 600 ml of hot ether. The organic layer was dried over magnesium sulfate and concentrated in vacuo to give 7.2 g of 2-chloro-4-methyl-6-methoxypyrimidine as a white, crystalline solid, m.p. 36°-38° C.
後処理
- additionadded over a period of 30-40 minutes
- filtrationThe precipitate was filtered
- extractionextracted thoroughly with approximately 600 ml of hot ether
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-94dc46d8fb8642d29412913bcd5a3a39
- 出典データセット
- uspto-grants-1986_01
- 特許番号
- US04565567
反応ノート
読み込み中…