Cesium carbonate → HCID 53380742、化合物

関与物質

役割	名称	HCID	仕込み量
反応物	Cesium carbonate	HCID 10796	—
反応物	4-(4-Chloropyrimidin-2-yl)morpholine	HCID 824643	—
反応物	N-Cyclopropyl-N'-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)urea	HCID 44119149	—
触媒	HCID 178418476	HCID 178418476	—
溶媒	1,4-Dioxane	HCID 31275	—
生成物	HCID 53380742	HCID 53380742	6%

反応手順

To a solution of 4-(4-chloropyrimidin-2-yl)morpholine (80 mg, 0.40 mmol) and (4-(3-cyclopropylureido)phenyl)boronic acid pinacol ester (145 mg, 0.48 mmol) in dioxane (2 mL) was added Pd(PPh3)2Cl2 (14 mg, 0.02 mmol) and Cs2CO3 (2M aq solution, 0.3 mL). The reaction mixture was then heated to reflux for 16 h. The crude reaction mixture was then partitioned between water and EtOAc, the phases separated and the organic layer washed with aqueous NaHCO3 and brine, dried over magnesium sulfate, filtered and the solvent removed in vacuo. The residue was purified by flash chromatography (0-5% EtOAc/MeOH) to yield a white solid (7.8 mg, 6%).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US09249129B2
出典データセット	uspto-grants-2016_02
ORD ID	ord-696307e215554ca484a981da7f3b5f94
出典メモ	uspto-grants-2016_02