Methyl iodide → 2,2,4-trimethyl-6-nitro-2H-1,4-benzoxazin-3(4H)-one
반응식
[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]1참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-084d1642d0904ad5a1a2113cf8258135
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08642624B2
반응 노트
불러오는 중…