HRID2227999

反应详情

EQUATION

反应方程式

HRID 2227999 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-fluoroacetophenone (8.8 ml, 72.4 mmol), paraformaldehyde (2.9 g, 94.1 mmol), dimethylamine hydrochloride (7.8 g, 96.78 mmol) conc. HCl (1 ml) in ethanol (10 ml) was heated under reflux for 3 hrs. The solution was added to acetone (50 ml), allowed to cool and placed in the fridge overnight. The resulting white solid was filtered washed with acetone (100 ml) and dried over P2O5 under vacuum to give 1-(4-fluorophenyl)-3-(N,N-dimethylamino)propanone hydrochloride 7.82 g, (51%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hrs
  3. temperatureto cool
  4. customplaced in the fridge overnight
  5. filtrationThe resulting white solid was filtered
  6. washwashed with acetone (100 ml)
  7. dry with materialdried over P2O5 under vacuum