Lawesson's reagent → 2,2-dimethyl-6-nitro-2H-benzo[b][1,4]oxazine-3(4H)-thione
반응식
[CH3:1][C:2]1([CH3:16])[O:7][C:6]2[CH:8]=[CH:9][C:10]([N+:12]([O-:14])=[O:13])=[CH:11][C:5]=2[NH:4][C:3]1=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:26])=CC=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:16])[O:7][C:6]2[CH:8]=[CH:9][C:10]([N+:12]([O-:14])=[O:13])=[CH:11][C:5]=2[NH:4][C:3]1=[S:26]참가 물질
4
실험 절차
2,2-Dimethyl-6-nitro-2H-benzo[b][1,4]oxazin-3(4H)-one (3.4 g) and Lawesson's reagent (6.19 g, 1.0 eq.) were suspended in toluene (100 ml). The reaction mixture was refluxed for one hour. The mixture was then evaporated. The residue was purified by Combiflash chromatography (EtOAc in hexanes=0-100%) to give 2,2-dimethyl-6-nitro-2H-benzo[b][1,4]oxazine-3(4H)-thione (3 g, 82% yield).
후처리
- temperatureThe reaction mixture was refluxed for one hour
- customThe mixture was then evaporated
- customThe residue was purified by Combiflash chromatography (EtOAc in hexanes=0-100%)
출처 및 근거
- ORD 기록
- ord-f7022769ef164b6e8225719bef8ba1ee
- 출처 데이터셋
- uspto-grants-2016_04
- 특허 번호
- US09321763B2
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