반응식
N(OC(C)(C)C)=[O:2].N[C:9]1[C:14]([O:15][CH3:16])=[C:13]([Cl:17])[CH:12]=[C:11]([F:18])[C:10]=1[N:19]1[C:24](=[O:25])[CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[N:21]([CH3:30])[C:20]1=[O:31].Cl>S([O-])([O-])(=O)=O.[Cu+2].[Cu-]=O.O.[N+]([O-])([O-])=O.[Cu+2].O.O.O.O.[N+]([O-])([O-])=O.[Cu+2].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.C(#N)C>[Cl:17][C:13]1[CH:12]=[C:11]([F:18])[C:10]([N:19]2[C:24](=[O:25])[CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[N:21]([CH3:30])[C:20]2=[O:31])=[C:9]([OH:2])[C:14]=1[O:15][CH3:16]참가 물질
반응물 3
생성물 1
시약·촉매·용매 4
실험 절차
An acetonitrile (10 ml) solution of copper (II) sulfate (0.52 g, 3.26 mmol), copper (I) oxide (0.47 g, 3.26 mmol) and copper (II) nitrate hemipentahydrate (0.76 g, 3.26 mmol) was stirred at −30° C., and added with tert-butyl nitrite (0.41 g, 3.97 mmol) and then an acetonitrile (3 ml) solution of 3-(2-amino-4-chloro-6-fluoro-3-methoxyphenyl)-1-methyl-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione (0.94 g, 2.56 mmol). After stirred for 16 hr (−30° C. to room temperature), the mixture was poured into cold 5% hydrochloric acid (30 ml) and then extracted with ethyl acetate (20 ml×3). The organic phase was washed with brine and dried over Na2SO4. Preparative TLC was used for purification (silica gel plates, 2000 microns, ether). Yield: 0.16 g, 0.44 mmol.
후처리
- extractionextracted with ethyl acetate (20 ml×3)
- washThe organic phase was washed with brine
- dry with materialdried over Na2SO4
- customPreparative TLC was used for purification (silica gel plates, 2000 microns, ether)
출처 및 근거
- ORD 기록
- ord-1957e37683444cdcbe5a1cf20c9e049f
- 출처 데이터셋
- uspto-grants-2002_03
- 특허 번호
- US06355799B1
연결된 노트
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