HRID60965

反应详情

EQUATION

反应方程式

HRID 60965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of ((2S,3R)-2-(aminomethyl)-3-methylpiperidin-1-yl)(5-methyl-2-(1-methyl-1H-pyrazol-4-yl)phenyl)methanone (80 mg, 245 μmol), 2-bromo-5-fluoropyridine (47 mg, 270 μmol), Pd2dba3 (5.0 mg, 4.9 μmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos; 4.2 mg, 7 μmol), and NaOtBu (35 mg, 368 μmol) in dioxane (2 mL) was purged with argon, and then stirred at 100° C. overnight. The reaction was cooled, filtered through a pad of silica gel and concentrated in vacuo. The crude reaction mixture was purified by reverse-phase preparative HPLC to afford the title compound. MS (ESI) 422 (M+H).

WORKUP

后处理

  1. customwas purged with argon
  2. temperatureThe reaction was cooled
  3. filtrationfiltered through a pad of silica gel
  4. concentrationconcentrated in vacuo
  5. customThe crude reaction mixture
  6. customwas purified by reverse-phase preparative HPLC