HCID 18957785, 화합물 → 6-Amino-3,4-dihydro-2,2-dioxo-4-oxo-1H-2,3-benzothiazine
반응식
[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]=1참가 물질
4
실험 절차
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).
후처리
- filtrationThe mixture was then filtered
- washthe solid washed with methanol
- customthe filtrates evaporated in vacuo
출처 및 근거
- ORD 기록
- ord-8254a5c208ae43858fcd8f0195485941
- 출처 데이터셋
- uspto-grants-1994_11
- 특허 번호
- US05360802
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