Acetic Acid → 2-Methylbenzo[d]thiazol-7-amine
反応式
[CH3:1][C:2]1[S:3][C:4]2[C:10]([N+:11]([O-])=O)=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.C(O)(=O)C>C(O)C.[Fe]>[CH3:1][C:2]1[S:3][C:4]2[C:10]([NH2:11])=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1参加物
5
実験手順
To a solution of 3.8 g of the product from Example 6 and 8.1 g of glacial acetic acid in 56 mL absolute ethanol at reflux temperature was added 3.8 g of iron powder in small portions. The reaction mixture was heated at reflux temperature for about 36 hours, and was then cooled and filtered. The filtrate was concentrated in vacuo and the residue treated with several mL cold water to give a solid. Filtration and drying gave 2.2 g of the title compound as a tan-colored solid, m.p. 100°-101° C.; NMR (CDCl3): δ 2.8 (3H, s), 3.9 (2H, br s), 6.65 (1H, d, J=8 Hz), 7.2 (1H, t, J=8 Hz), 7.5 (1H, d, J=8 Hz).
後処理
- temperatureThe reaction mixture was heated
- temperatureat reflux temperature for about 36 hours
- temperaturewas then cooled
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
- additionthe residue treated with several mL cold water
- customto give a solid
- filtrationFiltration
- customdrying
出典と根拠
- ORDレコード
- ord-ecdc24bb93914edc805b818fcc0a98c4
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04643759
反応ノート
読み込み中…