HRID321

反应详情

EQUATION

反应方程式

HRID 321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

3-Nitroaniline (140 mg, 1.01 mmol), 2,4-dichloropyridine (150 mg, 1.01 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (70.4 mg, 0.12 mmol) and cesium carbonate (660 mg, 2.03 mmol) were stirred in dioxane (5 mL). The mixture was purged with nitrogen for 10 minutes. Palladium(II) acetate (22.76 mg, 0.10 mmol) was added and the mixture heated at 100 °C for 1.5h. The mixture was cooled, filtered and concentrated. The crude product was purified by flash silica chromatography, eluting with 1% MeOH in DCM. Pure fractions were evaporated to dryness to afford 4-chloro-N-(3-nitrophenyl)pyridin-2-amine (121 mg, 47.8 %) as a yellow solid.