Isoamyl Nitrite → 7-Fluorobenzo[d]thiazole
反応式
[F:1][C:2]1[C:10]2[S:9][C:8](N)=[N:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.N(OCCC(C)C)=O>C1COCC1>[F:1][C:2]1[C:10]2[S:9][CH:8]=[N:7][C:6]=2[CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
To a solution of 7-fluorobenzo[d]thiazol-2-amine 25C (1 g, 5.95 mmol) in THF (10 mL) was added isoamyl nitrite (1.51 g, 12.9 mmol) at room temperature. After refluxing for 3 hr, the reaction mixture was then allowed to cool to room temperature and poured into ice water (50 mL), and then extracted with EtOAc. The organic extract was washed with water and brine, dried and evaporated. The residue was chromatographed on silica gel to get the 7-fluorobenzo[d]thiazole as colorless oil. LC-MS: m/z 154.2 (M+H)+
後処理
- temperatureAfter refluxing for 3 hr
- extractionextracted with EtOAc
- extractionThe organic extract
- washwas washed with water and brine
- customdried
- customevaporated
- customThe residue was chromatographed on silica gel
出典と根拠
- ORDレコード
- ord-96389c24297e4bccaedb277c2ae87532
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09108921B2
反応ノート
読み込み中…