HRID2380965

反应详情

EQUATION

反应方程式

HRID 2380965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-{[4-(4-Phenyl-piperazine-1-carbonyl)-phenylamino]-methyl}-benzonitrile (50 mg, 0.13 mmol), phenylsulfonylchloride (80 mg, 0.42 mmol) and pyridine (0.04 mL, 0.44 mmol) in dichloromethane (5 ml) was heated to reflux for 16 hours. The reaction mixture was cooled to room temperature and the quenched by the addition of water (4 ml). The organics were collected, dried over magnesium sulfate and concentrated in vacuo The residue was purified by preparative thin layer chromatography (dichloromethane/ethyl acetate 1:1) to afford the title compound as a white solid (16.4 mg, 27% yield). HPLC retention time 6.71 min. Mass spectrum (ES+) m/z 475 (M+H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 16 hours
  3. customthe quenched by the addition of water (4 ml)
  4. customThe organics were collected
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo The residue
  7. customwas purified by preparative thin layer chromatography (dichloromethane/ethyl acetate 1:1)