HRID1434945

反应详情

EQUATION

反应方程式

HRID 1434945 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

[4-(5-Bromo-thiophen-2-yl)-pyrimidin-2-yl]-(2,2,6,6-tetramethyl-piperidin-4-yl)-amine (Step C of Example 5, 100 mg, 0.253 mmol), 4-trimethylstannylpyridine (186 mg, 0.506 mol) and PdCl2(PPh3)2 (18 mg, 0.025 mmol) were dissolved in xylene (5 ml) and heated to 120° C. for 30 minutes. The reaction mixture was poured on 1N-NaOH and extracted three times with EtOAc. The combined organic phases were dried over sodium sulfate, filtered, evaporated to dryness and purified via preparative HPLC to give the title compound as yellow crystals. Yield: 23 mg (23%)

WORKUP

后处理

  1. extractionextracted three times with EtOAc
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated to dryness
  5. custompurified via preparative HPLC