Pyridine → 4-(4-methylpiperazin-1-ylaminomethyl)-N-[4-methyl-3-(4-(pyridin-3-yl)pyrimidin-2-yl)aminophenyl]benzamide

関与物質

役割	名称	HCID	仕込み量
反応物	Pyridine	HCID 1049	—
反応物	1-Amino-4-methylpiperazine	HCID 81349	—
反応物	4-(Chloromethyl)-N-(4-methyl-3-((4-(3-pyridinyl)-2-pyrimidinyl)amino)phenyl)benzamide	HCID 10181075	—
溶媒	Tetrahydrofuran	HCID 8028	—
生成物	4-(4-methylpiperazin-1-ylaminomethyl)-N-[4-methyl-3-(4-(pyridin-3-yl)pyrimidin-2-yl)aminophenyl]benzamide	HCID 9892492	74.3%

反応手順

N-[5-(4-chloromethylbenzoylamino)-2-methylphenyl]-4-(3-pyridyl)-2-pyrimidine-amine (1 g, 2.33 mmol) was dissolved in tetrahydrofuran (20 ml), pyridine (360 μl, 4.66 mmol) was added thereto, and the mixture was stirred for 30 minutes. 1-Amino-4-methylpiperazine (418 μl, 3.49 mmol) was added, and the mixture was refluxed for 12 hours and filtered. The filtrate was concentrated, subjected to column chromatography (eluent: chloroform:methanol=3:1(v/v)), concentrated again, and then crystallized from dimethylether to give 4-(4-methylpiperazin-1-ylaminomethyl)-N-[4-methyl-3-(4-(pyridin-3-yl)pyrimidin-2-yl)aminophenyl]benzamide (880 mg).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07595323B2
出典データセット	uspto-grants-2009_09
ORD ID	ord-5fb5e89c521b4645b33ae7314b121fb4
出典メモ	uspto-grants-2009_09