戻る
化工社化工社 化学情報印刷レポート · 研究参考用
HRID 2089631作成日:2026年10月27日

Dimethylformamide → HCID 68212999、化合物

https://huagongshe.com/reaction/2089631

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Cesium carbonateHCID 10796—
反応物3-Methoxy-2,2-dimethylpropionic acid chloromethyl esterHCID 14459693—
反応物N-[1-amino-1-(4-{[[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}phenyl)methylidene]benzamideHCID 136334022—
溶媒WaterHCID 962—
溶媒Ethyl AcetateHCID 8857—
生成物HCID 68212999HCID 6821299935.8%

反応条件

温度60 °C

反応手順

To a mixture of N-[1-amino-1-(4-{[[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]-(5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-[1,2,4]triazol-3-yl)methyl]amino}phenyl)methylidene]benzamide (Example 1a, 45 mg) and DMF (2 mL), cesium carbonate (29 mg) and 3-methoxy-2,2-dimethylpropionic acid chloromethyl ester (20 mg) were sequentially added, and the resulting mixture was stirred at 60° C. for 4 hours. The resulting mixture was poured into ethyl acetate (30 mL) and water (20 mL). After shaking the mixture, the organic layer was collected. The organic layer was sequentially washed twice with water (30 mL) and with saturated aqueous sodium chloride solution (20 mL), and dried over anhydrous magnesium sulfate. The resulting mixture was filtered, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by NAM silica gel column chromatography (mixed solvent of methanol-ethyl acetate) to obtain the captioned compound (20 mg).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08436009B2
出典データセットuspto-grants-2013_05
ORD IDord-527ceb6ba360489dacf24700108e7804
出典メモuspto-grants-2013_05