반응식
Cl[CH:2]1[C:11]2[C:6](=[C:7]([O:12][C:13]3[N:18]=[C:17]([O:19][CH3:20])[CH:16]=[C:15]([O:21][CH3:22])[N:14]=3)[CH:8]=[CH:9][CH:10]=2)[C:4](=[O:5])[O:3]1.[F-:23].[K+].C1OCCOCCOCCOCCOCCOC1>>[CH3:22][O:21][C:15]1[CH:16]=[C:17]([O:19][CH3:20])[N:18]=[C:13]([O:12][C:7]2[CH:8]=[CH:9][CH:10]=[C:11]3[C:6]=2[C:4](=[O:5])[O:3][CH:2]3[F:23])[N:14]=1참가 물질
4
실험 절차
A mixture of 1.0 g of 3-chloro-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see Example 85) and 0.19 g of spray-dried potassium fluoride and a spatula tip of 18-crown-6 is heated at reflux temperature for 100 minutes. The mixture is then filtered over Celite® and is concentrated by evaporation, and the crude product is recrystallised from ethyl acetate/n-hexane to yield 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-fluoro-phthalide, m.p. 172°-174° C.
후처리
- temperatureat reflux temperature for 100 minutes
- filtrationThe mixture is then filtered over Celite®
- concentrationis concentrated by evaporation
- customthe crude product is recrystallised from ethyl acetate/n-hexane
출처 및 근거
- ORD 기록
- ord-fa7b0110ae764beba36ccd7ed7b688fd
- 출처 데이터셋
- uspto-grants-1995_06
- 특허 번호
- US05428002
연결된 노트
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