HRID2065751

反应详情

EQUATION

反应方程式

HRID 2065751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of [4-(2,5-dimethyl-phenyl)-piperazin-1-yl]-[1-(4-fluoro-2-methyl-phenyl)-piperazin-2-yl]-methanone hydrochloride (42 mg) in DMF (1 mL) was added 3-methoxybenzene sulfonyl chloride (21.4 mg) and triethyl amine (40 μL). The reaction mixture was stirred at ambient temperature for 2 h, was diluted with ethyl acetate and washed with a saturated aqueous solution of NaHCO3. The combined organic phases were washed with water and brine, dried (Na2SO4), filtered and evaporated. The crude product was purified by column chromatography (SiO2, n-heptane/ethyl acetate 2:1) to give [4-(2,5-dimethyl-phenyl)-piperazin-1-yl]-[1-(4-fluoro-2-methyl-phenyl)-4-(3-methoxy-benzenesulfonyl)-piperazin-2-yl]-methanone (42 mg) as white solid, MS: 581.3 ([M+H]+).

WORKUP

后处理

  1. washwashed with a saturated aqueous solution of NaHCO3
  2. washThe combined organic phases were washed with water and brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe crude product was purified by column chromatography (SiO2, n-heptane/ethyl acetate 2:1)