Bromine → HCID 89655859、化合物
反応式
[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8](=[O:11])[NH:9][CH:10]=1)(=[O:4])=[O:3].C([O-])(=O)C.[Na+].[Br:17]Br>C(O)(=O)C>[Br:17][C:7]1[C:8](=[O:11])[NH:9][CH:10]=[C:5]([S:2]([CH3:1])(=[O:4])=[O:3])[CH:6]=1参加物
5
反応条件
- 温度
- 40 °C
実験手順
To a solution of Example 288c (0.671 g, 3.87 mmol) and sodium acetate (0.318 g, 3.87 mmol) in acetic acid (8.50 mL) was added bromine (0.201 mL, 3.91 mmol) dropwise as a solution in acetic acid (1.7 mL). The reaction mixture was stirred at 40° C. for 3 hours. Bromine (0.05 mL) was added, and the reaction mixture was stirred at 40° C. for 2 hours. The reaction mixture was cooled to ambient temperature and quenched with 100 mL of 10% aqueous sodium thiosulfate. The resulting suspension was filtered, and the solid collected and dried for 16 hours to provide the title compound (0.64 g, 66%).
後処理
- stirringthe reaction mixture was stirred at 40° C. for 2 hours
- temperatureThe reaction mixture was cooled to ambient temperature
- customquenched with 100 mL of 10% aqueous sodium thiosulfate
- filtrationThe resulting suspension was filtered
- customthe solid collected
- customdried for 16 hours
出典と根拠
- ORDレコード
- ord-f14a66215ab945fcb59be10991922590
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296741B2
反応ノート
読み込み中…