Hydrochloric Acid → HCID 13648719、化合物
反応式
[C:1]([N:5]1[C:10](=[O:11])[C:9]([Br:12])=[C:8](Br)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[SH-:14].[Na+].Cl>O>[C:1]([N:5]1[C:10](=[O:11])[C:9]([Br:12])=[C:8]([SH:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]参加物
5
反応条件
- 温度
- 60 °C
実験手順
To 200 ml of water were added 31.0 g of 2-tert.-butyl-4,5-dibromo-3(2H)-pyridazinone and 15.8 g of 70% sodium hydrosulfide. After stirring at 60° C. for 4 hours, the resulting mixture was allowed to cool to room temperature and incorporated with about 8 ml of concentrated hydrochloric acid to lower the pH of the liquid to not higher than 2. The resulting solid was filtered off, washed with water, dried and then recrystallized from benzene/n-hexane to give 8.0 g of the intended product as white crystals of m.p. 107°-110° C. (yield: 30.4%).
後処理
- filtrationThe resulting solid was filtered off
- washwashed with water
- customdried
- customrecrystallized from benzene/n-hexane
出典と根拠
- ORDレコード
- ord-48e0a2d377c7479c9e644d004df6c49c
- 出典データセット
- uspto-grants-1989_10
- 特許番号
- US04877787
反応ノート
読み込み中…