Ammonia → 6-Bromo-1,2,4-triazine-3,5(2H,4H)-dione
反応式
[N:1]1[NH:2][C:3](=[O:8])[NH:4][C:5](=[O:7])[CH:6]=1.[Br:9]Br.N>O>[Br:9][C:6]1[C:5](=[O:7])[NH:4][C:3](=[O:8])[NH:2][N:1]=1参加物
5
実験手順
2H-[1,2,4]triazin-3,5-dione (50 g, 442 mmol) is placed in the presence of 60 ml of bromine in 800 ml of water at 60° C. for 10 h. The reaction medium is then slowly added to an ammonia solution until pH=5. It is then extracted in ethyl acetate and the organic phases are dried on MgSO4. After filtration and dry concentration, 1a is isolated in the form of a white solid (79.2 g, yield=93%). TLC silica gel 60 F 254 Merck, CH2Cl2:MeOH 90:10, Rf=0.32.
後処理
- extractionIt is then extracted in ethyl acetate
- customthe organic phases are dried on MgSO4
- filtrationAfter filtration
- customdry
- concentrationconcentration
出典と根拠
- ORDレコード
- ord-bbacedb8625749678ef53f6a6b65ac50
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07713971B2
反応ノート
読み込み中…