HRID2045914

反应详情

EQUATION

反应方程式

HRID 2045914 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A slurry of 2-chloro-N-(3-quinoxalin-2-ylphenyl)acetamide (100 mg, 0.336 mmol), 1-(4-chlorophenyl)piperazine dihydrochloride (100 mg, 0.367 mmol) and K2CO3 (149 mg, 1.075 mmol) in MeCN (5 mL) was heated at reflux for 24 hrs. The reaction mixture was diluted with ethyl acetate (20 mL), and the organic phase washed with water (20 mL) and then brine (20 mL), dried over MgSO4 and evaporated in vacuo. The residue was triturated with diethyl ether and dried in vacuo at 50° C. to afford 2-[4-(4-chlorophenyl)piperazin-1-yl]-N-(3-(quinoxalin-2-yl)phenyl)acetamide (56 mg, 36% yield). LCMS calculated for C26H24ClN5O (M+H): 458.17. found 458.21. 1H-NMR (DMSO-d6, 400 Mhz) δH: 10.00 (1H, br. s), 9.51 (1H, s), 8.55 (1H, m), 8.15-8.10 (2H, m), 8.05 (1H, d, 1=7.5 Hz), 7.95-7.80 (3H, m), 7.55 (1H, m), 7.21 (2H, d, J=7.5 Hz), 6.90 (2H, d, J=7.5 Hz), 3.21 (4H, m), 2.61 (4H, m).

WORKUP

后处理

  1. temperatureat reflux for 24 hrs
  2. washthe organic phase washed with water (20 mL)
  3. dry with materialbrine (20 mL), dried over MgSO4
  4. customevaporated in vacuo
  5. customThe residue was triturated with diethyl ether
  6. customdried in vacuo at 50° C.