HRID629008

反应详情

EQUATION

反应方程式

HRID 629008 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 4-(2,6-dichloro-5-methylsulfanyl-pyrimidin-4-yl)-morpholine (200 mg, 0.71 mmol.), 4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-aniline) (172.0 mg, 0.781 mmol.), (PPh3)4Pd (437 mg, 0.07 mmol.), 2M Na2CO3 (1.0 ml, 2.13 mmol, 3.0 eq.) and dioxane (15.0 ml) was added to the reaction vessel which was flushed with argon. The reaction mixture was stirred at 90° C. for 12 hrs and then dried so that the solvent was evaporated. The reaction mixture was partitioned between EA and water. The organic layers were collected, washed with brine, dried over MgSO4, filtered and evaporated in vacuo. The resulting residue was purified by flash chromatography on silica gel (Hexane/EtOAc 3:2) to give a pale yellow solid of 102 mg (42.3%).

WORKUP

后处理

  1. additionwas added to the reaction vessel which
  2. customwas flushed with argon
  3. customdried so that the solvent
  4. customwas evaporated
  5. customThe reaction mixture was partitioned between EA and water
  6. customThe organic layers were collected
  7. washwashed with brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated in vacuo
  11. customThe resulting residue was purified by flash chromatography on silica gel (Hexane/EtOAc 3:2)
  12. customto give a pale yellow solid of 102 mg (42.3%)