Lawesson's reagent → 2,2-dimethyl-6-nitro-2H-benzo[b][1,4]oxazine-3(4H)-thione
反応式
[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]参加物
4
実験手順
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).
後処理
- 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%)
出典と根拠
- ORDレコード
- ord-f7022769ef164b6e8225719bef8ba1ee
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09321763B2
反応ノート
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