反応式
C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.[NH2:47][C:48]1[CH:53]=[CH:52][N:51]=[CH:50][C:49]=1[F:54].C([O-])([O-])=O.[Cs+].[Cs+].N(Cl)Cl.Cl[C:65]1[C:66]2[CH:82]=[CH:81][CH:80]=[N:79][C:67]=2[N:68]=[C:69]([C:71]2[CH:76]=[C:75]([Cl:77])[CH:74]=[CH:73][C:72]=2[F:78])[N:70]=1>CC([O-])=O.CC([O-])=O.[Pd+2].O1CCOCC1>[Cl:77][C:75]1[CH:74]=[CH:73][C:72]([F:78])=[C:71]([C:69]2[N:70]=[C:65]([NH:47][C:48]3[CH:53]=[CH:52][N:51]=[CH:50][C:49]=3[F:54])[C:66]3[CH:82]=[CH:81][CH:80]=[N:79][C:67]=3[N:68]=2)[CH:76]=1参加物
8
反応物 5
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 110 °C
実験手順
To a suspension of dioxane (5 ml), Pd(OAc)2 (50 mg), BINAP (20 mg), 4-amino-3-fluoro-pyridine (42 mg) and Cs2CO3 (200 mg) was added the crude imino chloride, 4-Chloro-2-(5-Chloro-2-fluoro-phenyl)-pyrido[2,3-d]pyrimidine (100 mg, 0.34 mmol) in a sealed tube. The reaction mixture was heated to 110° C. for 15 h. The reaction mixture was cooled to r.t. and filtered through Celite® and the crude material was purified by silica gel flash column chromatography (95% to 5% gradient CH2Cl2/EtOAc) to afford [2-(5-Chloro-2 -fluoro-phenyl)-pyrido[2,3-d]pyrimidin-4-yl]-(3-fluoro-pyridin-4-yl)-amine (27.3 mg).
後処理
- temperatureThe reaction mixture was cooled to r.t.
- filtrationfiltered through Celite®
- customthe crude material was purified by silica gel flash column chromatography (95% to 5% gradient CH2Cl2/EtOAc)
出典と根拠
- ORDレコード
- ord-f160a7ac685243b48eb237fa92fb6276
- 出典データセット
- uspto-grants-2007_06
- 特許番号
- US07232824B2
関連ノート
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