HRID2380964

反应详情

EQUATION

反应方程式

HRID 2380964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a stirred solution of (4-amino-phenyl)-(4-phenyl-piperazin-1-yl)-methanone (0.5 g, 1.78 mmol) in tetrahydrofuran (10 mL) was added 4-cyanobenzaldehyde (0.4 g, 2.67 mmol) followed by sodium borohydride and the reaction was heated to 50° C. for 2 hours. On cooling, the reaction was quenched by the addition of water (10 mL) and the aqueous solution basified by the addition of ammonium chloride (˜pH 8). The aqueous mixture was extracted using dichloromethane (3×10 ml) and the organic extracts combined, dried over magnesium sulfate and concentrated in vacuo to afford the title compound as an off white solid (604 mg, 98% yield). HPLC retention time 7.17 min. Mass spectrum (ES+) m/z 397 (M+H).

WORKUP

后处理

  1. temperatureOn cooling
  2. customthe reaction was quenched by the addition of water (10 mL)
  3. additionthe aqueous solution basified by the addition of ammonium chloride (˜pH 8)
  4. extractionThe aqueous mixture was extracted
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo