Hydrochloric Acid → 7-Fluoro-1,3-benzothiazol-2-amine
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-])=O)[C:3]=1[S:11][C:12]#[N:13].C(O)C.Cl>O>[F:1][C:2]1[C:3]2[S:11][C:12]([NH2:13])=[N:8][C:4]=2[CH:5]=[CH:6][CH:7]=1参加物
5
実験手順
A mixture of 1-fluoro-3-nitro-2-thiocyanatobenzene 2 (3.96 g, 0.02 mol), ethanol (30 mL), water (25 mL) and conc. hydrochloric acid (25 mL) was refluxed gently during the addition of hydrogen-reduced iron powder (8 g). After refluxing for 16 hr, the liquor was filtered hot, cooled, the residue filtered, dissolved in hot water, and neutralized with ammonia and then extracted with EtOAc to get the compound 7-fluorobenzo[d]thiazol-2-amine (1 g) as a colorless oil. LC-MS: m/z 169.2 (M+H)+
後処理
- temperatureAfter refluxing for 16 hr
- filtrationthe liquor was filtered hot
- temperaturecooled
- filtrationthe residue filtered
- dissolutiondissolved in hot water
- extractionextracted with EtOAc
出典と根拠
- ORDレコード
- ord-9ea32e9d4cb2489ea1c7a9824bd613c8
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09365545B2
反応ノート
読み込み中…