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4-Methylmorpholine → N-[5-(5-chloro-2-methylbenzoxazol-6-yl)phenyl](3-fluoro(4-pyridyl))carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 2-Chloro-4,6-dimethoxy-1,3,5-triazine | HCID 18450 | — |
| 反応物 | 3-Fluoropyridine-4-carboxylic acid | HCID 345361 | — |
| 反応物 | 4-(5-Chloro-2-methylbenzoxazol-6-yl)phenylamine | HCID 67467295 | — |
| 反応物 | Sodium bicarbonate ethyl acetate | HCID 86584982 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[5-(5-chloro-2-methylbenzoxazol-6-yl)phenyl](3-fluoro(4-pyridyl))carboxamide | HCID 67468423 | 95.7% |
反応手順
A suspension of 3-fluoroisonicotinic acid (20 mg, 0.14 mmol), 2-chloro-4,6-dimethoxy-1,3,5-triazine (CDMT) (28 mg, 0.16 mmol) and 40 μl N-methyl morpholine in 1 ml DCM was stirred at r.t. for 1 h before addition of 56 (20 mg, 0.078 mmol). The resulting reaction mixture was stirred at r.t. for overnight. The reaction mixture was worked up with aq. NaHCO3/EA. Org. phase was washed with brine, concentrated, subjected to silica flash column chromatography to furnish 28.5 mg title compound 60 as off-white solid. (Yield: 95.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754219B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-88aed97be0df4e2c8b6be259ac849e52 |
| 出典メモ | uspto-grants-2014_06 |