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1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) → {4-[2-(2-Fluoro-5-trifluoromethyl-phenyl)-[1,8]naphthyridin-4-ylamino]-pyridin-3-yl}-methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | 4-Aminopyridine-3-methanol | HCID 10796739 | — |
| 反応物 | 4-Chloro-2-(2-fluoro-5-trifluoromethyl-phenyl)-[1,8]naphthyridine | HCID 53344725 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | {4-[2-(2-Fluoro-5-trifluoromethyl-phenyl)-[1,8]naphthyridin-4-ylamino]-pyridin-3-yl}-methanol | HCID 53372195 | 31% |
反応手順
150 mg 4-chloro-2-(2-fluoro-5-trifluoromethyl-phenyl)-[1,8]naphthyridine and 57 mg 4-amino-3-hydroxymethylpyridine in 6 ml dioxane containing 299 mg Cs2CO3, 8 mg Pd2 (dba)3 and 10 mg xantphos were incubated under argon gas at 90° C. for 18 hrs. After evaporation to dryness the crude sample was flashed on SiO2 with a MeOH gradient in DCM. A pooled fraction was evaporated to give 59 mg product {4-[2-(2-fluoro-5-trifluoromethyl-phenyl)-[1,8]naphthyridin-4-ylamino]-pyridin-3-yl}-methanol with Rt˜1.48 min and correct mass found M+H˜415.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08815893B2 |
| 出典データセット | uspto-grants-2014_08 |
| ORD ID | ord-c358abf462c0423dacadf29d80fb090b |
| 出典メモ | uspto-grants-2014_08 |