HRID2090299

反应详情

EQUATION

反应方程式

HRID 2090299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 4-(7-bromo-3,4-dihydroisoquinolin-2(1H)-yl)-6-(4-methylpiperazin-1-yl)pyrimidin-2-amine (20.0 mg, 0.0496 mmol), 6-methyl-2-pyridinamine, (8.04 mg, 0.0744 mmol, Aldrich, Cat. No. A75706), a solution of potassium tert-butoxide in tetrahydrofuran (0.0992 mL, 0.0992 mmol, 1.00 M, Aldrich Cat. 328650), palladium acetate (0.445 mg, 0.00198 mmol, Aldrich, Cat. No. 379875), and 2-[dicyclohexylphosphino]biphenyl (0.869 mg, 0.00248 mmol, Aldrich, Cat. No. 638099) in 1,4-dioxane (1 mL) was degassed with nitrogen and then heated at 120° C. for 16 hours. The reaction mixture was cooled to r.t. and concentrated. Then the reaction mixture was dissolved in MeOH and purified by RP-HPLC (pH=10) to afford the desired compound. LCMS(M+H)+: m/z=431.4.

WORKUP

后处理

  1. custom638099) in 1,4-dioxane (1 mL) was degassed with nitrogen
  2. temperatureThe reaction mixture was cooled to r.t.
  3. concentrationconcentrated
  4. dissolutionThen the reaction mixture was dissolved in MeOH
  5. custompurified by RP-HPLC (pH=10)