反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:22])[C:7]=1[S:8][C:9]1[S:13][C:12]([C:14]([O:16]CC)=[O:15])=[CH:11][C:10]=1[N+:19]([O-:21])=[O:20].S(=O)(=O)(O)O>O>[Cl:22][C:6]1[CH:5]=[N:4][CH:3]=[C:2]([Cl:1])[C:7]=1[S:8][C:9]1[S:13][C:12]([C:14]([OH:16])=[O:15])=[CH:11][C:10]=1[N+:19]([O-:21])=[O:20]参加物
4
反応条件
- 温度
- 100 °C
実験手順
Ethyl 5-[(3,5-dichloro-4-pyridyl)sulfanyl]-4-nitro-thiophene-2-carboxylate (1.8 g, 4.74 mmol) was added to a solution of concentrated sulfuric acid (10 mL) diluted with water (20 mL), and the resulting mixture was heated at 100° C. for 5 hours. After this time, the mixture was poured into ice (4.5 mL) and stirred at room temperature for 20 minutes, then the resulting solid was collected by filtration, washed with water and dried in vacuo at 40° C. overnight to afford the title product as a white solid (1.3 g, 78% yield). 1H NMR (400 MHz, d6-DMSO) δ: 9.0 (2H, s), 8.1 (1H, s). MS m/z: 350.85, 352.90 [M+H]+.
後処理
- filtrationthe resulting solid was collected by filtration
- washwashed with water
- customdried in vacuo at 40° C. overnight
出典と根拠
- ORDレコード
- ord-31fe241f358849b38de6d3b4dd6f088e
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08680139B2
関連ノート
読み込み中…