HCID 18957785、化合物 → 6-Amino-3,4-dihydro-2,2-dioxo-4-oxo-1H-2,3-benzothiazine
反応式
[O:1]=[S:2]1(=[O:16])[NH:7][C:6](=[O:8])[C:5]2[CH:9]=[C:10]([N+:13]([O-])=O)[CH:11]=[CH:12][C:4]=2[CH2:3]1>[Pd].CO>[NH2:13][C:10]1[CH:11]=[CH:12][C:4]2[CH2:3][S:2](=[O:16])(=[O:1])[NH:7][C:6](=[O:8])[C:5]=2[CH:9]=1参加物
4
実験手順
A mixture of 3,4-dihydro-2,2-dioxo-6-nitro-4-oxo-1H-2,3-benzothiazine (267 mg, 1.1 mmol) and 10% palladium on carbon (26 mg, 10% (w/w)) in methanol (50 ml) was hydrogenated at 50 psi for 30 min. The mixture was then filtered, the solid washed with methanol and the filtrates evaporated in vacuo to give the title compound (239 mg, 100%) as a yellow solid. 1H NMR (360 MHz, D6-DMSO) δ 3.87 (2H, s), 5.11 (2H, brs), 6.59 (1H, dd, J=8.0 and 2.5 Hz), 6.88 (1H, d, J=8.0 Hz), 7.15 (1H, d, J=2.5 Hz). MS (FAB) 211 (M-1).
後処理
- filtrationThe mixture was then filtered
- washthe solid washed with methanol
- customthe filtrates evaporated in vacuo
出典と根拠
- ORDレコード
- ord-8254a5c208ae43858fcd8f0195485941
- 出典データセット
- uspto-grants-1994_11
- 特許番号
- US05360802
反応ノート
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