Methyl iodide → 2,2,4-trimethyl-6-nitro-2H-1,4-benzoxazin-3(4H)-one
反応式
[CH3:1][C:2]1([CH3:16])[C:7](=[O:8])[NH:6][C:5]2[CH:9]=[C:10]([N+:13]([O-:15])=[O:14])[CH:11]=[CH:12][C:4]=2[O:3]1.CI.[C:19]([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:1][C:2]1([CH3:16])[C:7](=[O:8])[N:6]([CH3:19])[C:5]2[CH:9]=[C:10]([N+:13]([O-:15])=[O:14])[CH:11]=[CH:12][C:4]=2[O:3]1参加物
5
実験手順
2,2-Dimethyl-6-nitro-4H-benzo[1,4]oxazin-3-one (1.1 g) was mixed with MeI (850 mg, Aldrich), K2CO3 (1.38 g, Aldrich) and DMF (30 ml, Aldrich) at 40° C. for 48 h. The DMF was removed in vacuo and the residue was diluted with EtOAc (80 ml). The organic phase was washed with H2O (50 ml), aqueous Na2SO3 (50 ml) and brine (50 ml). The resulting solution was dried (MgSO4) and concentrated to provide the compound which was used as is.
後処理
- customThe DMF was removed in vacuo
- additionthe residue was diluted with EtOAc (80 ml)
- washThe organic phase was washed with H2O (50 ml), aqueous Na2SO3 (50 ml) and brine (50 ml)
- dry with materialThe resulting solution was dried (MgSO4)
- concentrationconcentrated
- customto provide the compound which
出典と根拠
- ORDレコード
- ord-084d1642d0904ad5a1a2113cf8258135
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642624B2
反応ノート
読み込み中…