HRID1522634

反应详情

EQUATION

反应方程式

HRID 1522634 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (60.0 mg, 0.104 mmol), 7-iodo-1-(4-methoxybenzyl)-1H-pyrazolo[4,3-b]pyridine (757 mg, 2.073 mmol), Pd2(dba)3 (95 mg, 0.104 mmol), 3′-fluoro-6′-methyl-2,2′-bipyridin-4-amine (421 mg, 2.073 mmol) and sodium 2-methylpropan-2-olate (598 mg, 6.22 mmol) were combined in dioxane (15 mL) and the mixture was heated at 110° C. for 10 minutes and then at 70° C. over night. The reaction was then cooled and concentrated to give a residue which was loaded onto silica and purified by column chromatography eluting with MeOH in CHCL3 (0-15%) to give N-(3′-fluoro-6′-methyl-2,2′-bipyridin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazolo[4,3-b]pyridin-7-amine and N-(3′-fluoro-6′-methyl-2,2′-bipyridin-4-yl)-2-(4-methoxybenzyl)-2H-pyrazolo[4,3-b]pyridin-7-amine as solid. MS [M+H] found 441.2.

WORKUP

后处理

  1. waitat 70° C. over night
  2. temperatureThe reaction was then cooled
  3. concentrationconcentrated
  4. customto give a residue which
  5. custompurified by column chromatography
  6. washeluting with MeOH in CHCL3 (0-15%)