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HRID 241840作成日:2026年10月27日

1,4-Dioxane → 5,6,7,8-Tetrahydro-6-(5-methylpyridin-2-yl)pyrido[4,3-d]pyrimidin-4(3H)-one

https://huagongshe.com/reaction/241840

反応式

関与物質

役割名称HCID仕込み量
反応物1,4-DioxaneHCID 31275—
反応物DiisopropylethylamineHCID 81531—
反応物2-Chloro-5-methyl-pyridineHCID 581393—
反応物5,6,7,8-Tetrahydropyrido[4,3-d]pyrimidin-4(3H)-oneHCID 135627628—
溶媒DimethylacetamideHCID 31374—
溶媒Chloroform isopropyl alcoholHCID 21906603—
生成物5,6,7,8-Tetrahydro-6-(5-methylpyridin-2-yl)pyrido[4,3-d]pyrimidin-4(3H)-oneHCID 13597895748.5%

反応条件

温度150 °C

反応手順

Into a 20 mL microwave tube was combined 5,6,7,8-tetrahydro-3H-pyrido[4,3-d]pyrimidin-4-one (0.280 g, 1.83 mmol), 2-chloro-5-methylpyridine (0.47 g, 3.7 mmol), 1,4-dioxane (2.5 mL), N,N-diisopropylethylamine (0.64 mL, 3.7 mmol) and N,N-dimethylacetamide (0.5 mL). The mixture was heated via microwave at 150° C. for 4 hours. The mixture was reduced in vacuo and taken up in chloroform:IPA (3:1) (50 mL). The organic phase was washed with sodium bicarbonate and brine (1×50 mL), dried over sodium sulfate, and reduced in vacuo. The residue was purified by flash chromatography on silica gel (0-10% methanol/methylene chloride) to give a bright yellow solid (0.215 g, 47.9%). MS: 243.3 [M+1]+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08653091B2
出典データセットuspto-grants-2014_02
ORD IDord-ee487f9731e740129df005f175727be1
出典メモuspto-grants-2014_02