HRID509267

反应详情

EQUATION

反应方程式

HRID 509267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1-Bromo-4-(methylsulfonyl)benzene (275 mg, 1.169 mmol), piperazine (302 mg, 3.507 mmol), Pd2(dba)3 (21 mg, 0.023 mmol), BINAP (44 mg, 0.070 mmol), and sodium-tert-butoxide (169 mg, 1.754 mmol) were suspended in toluene (5 ml), and then the resulting liquid was stirred at 100° C. under nitrogen stream for 15 hours. Distilled water (15 ml) was added to the resulting reaction liquid, followed by extraction with MC (20 ml×3). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (15% MeOH/MC), to obtain 56 mg of pale yellow solid (20%).

WORKUP

后处理

  1. extractionfollowed by extraction with MC (20 ml×3)
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfollowed by filtration and concentration
  4. customthe residue thus obtained