HRID1505628

反应详情

EQUATION

反应方程式

HRID 1505628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

4-Bromothiophenecarboxaldehyde (2.5 g, 13.1 mmol) was placed in a 25 ml round bottomed flask and charged with piperidine (0.14 ml, 0.11 mmol) and pyridine (7.1 ml). Malonic acid was then added (2.21 mg, 21.2 mmol) and the reaction heated to 100° C. and maintained for 24 h. The reaction was then allowed to cool to room temperature and the solvent removed in vacuo. The remaining residue was acidified with concentrated HCl to pH 3 and the solid collected, filtered and washed with distilled water (20 ml). It was then air and oven dried to yield a yellow solid (3.04 g, 100%).

WORKUP

后处理

  1. temperaturemaintained for 24 h
  2. temperatureto cool to room temperature
  3. customthe solvent removed in vacuo
  4. customthe solid collected
  5. filtrationfiltered
  6. washwashed with distilled water (20 ml)
  7. customair and oven dried