Bromine → 4-Bromo-6-chloro-5-methylpyridazin-3-amine
反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][C:3]=1[CH3:9].ClC1N=NC(N)=C(C)C=1.C([O-])(O)=O.[Na+].[Br:24]Br>CO.CCOC(C)=O>[Br:24][C:4]1[C:3]([CH3:9])=[C:2]([Cl:1])[N:7]=[N:6][C:5]=1[NH2:8]参加物
7
実験手順
The mixture of 6-chloro-5-methylpyridazin-3-amine and 3-chloro-5-methylpyridazin-6-amine (1.45 g, 10 mmol) from 1a and NaHCO3 (2.1 g, 25 mmol) were suspended in MeOH (20 mL) and treated with Br2 (0.57 mL, 11 mmol). The mixture was stirred at room temperature for 4 h, then filtered. The filtrate was condensed in vacuo. The resulting residue was resuspended in EtOAc (100 mL) and washed sequentially with sat. aqueous NaHCO3 solution (2×20 mL) and aqueous NaCl solution (1×20 mL). The solution was dried over MgSO4. The solvent was removed in vacuo to give crude 4-bromo-6-chloro-5-methylpyridazin-3-amine (1 g).
後処理
- filtrationfiltered
- customcondensed in vacuo
- washwashed sequentially with sat. aqueous NaHCO3 solution (2×20 mL) and aqueous NaCl solution (1×20 mL)
- dry with materialThe solution was dried over MgSO4
- customThe solvent was removed in vacuo
出典と根拠
- ORDレコード
- ord-e3c58a78953b4cfb8d08e35ebd2f641b
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07723336B2
反応ノート
読み込み中…