Cesium carbonate → 2-Chloro-5-methyl-N-(2,3-dimethylphenyl)pyrimidin-4-amine

関与物質

役割	名称	HCID	仕込み量
反応物	Cesium carbonate	HCID 10796	—
反応物	3-Bromo-o-xylene	HCID 68472	—
反応物	1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)	HCID 636044	—
反応物	2-Chloro-5-methylpyrimidin-4-amine	HCID 4302175	—
触媒	Bis(dibenzylideneacetone)palladium	HCID 9811564	—
溶媒	1,4-Dioxane	HCID 31275	—
生成物	2-Chloro-5-methyl-N-(2,3-dimethylphenyl)pyrimidin-4-amine	HCID 57516494	—

反応手順

A mixture of 2-chloro-5-methylpyrimidin-4-amine (143.6 mg, 1 mmol), 1-bromo-2,3-dimethylbenzene (222 mg, 1.2 mmol), Pd2(dba)3 (92 mg, 0.1 mmol), Xantphos (174 mg, 0.3 mmol) and cesium carbonate (1.3 g, 4 mmol) were suspended in dioxane (150 mL) and heated at reflux under the argon atmosphere for 20 h. The mixture was filtered and the filtrate concentrated in vacuo. The residue was dissolved in EtOAc (10 mL) and added hexanes (100 mL). The solid was collected by filtration and washed with hexanes to afford the crude title compound as a yellow solid.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07528143B2
出典データセット	uspto-grants-2009_05
ORD ID	ord-e0392a607bb54fb0805e8fbac196b555
出典メモ	uspto-grants-2009_05