Hydrochloric Acid → 7-Fluoro-1,3-benzothiazol-2-amine
반응식
[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]=1참가 물질
5
실험 절차
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)+
후처리
- temperatureAfter refluxing for 16 hr
- filtrationthe liquor was filtered hot
- temperaturecooled
- filtrationthe residue filtered
- dissolutiondissolved in hot water
- extractionextracted with EtOAc
출처 및 근거
- ORD 기록
- ord-9ea32e9d4cb2489ea1c7a9824bd613c8
- 출처 데이터셋
- uspto-grants-2016_06
- 특허 번호
- US09365545B2
반응 노트
불러오는 중…