HRID239715

反应详情

EQUATION

反应方程式

HRID 239715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-(4-chlorophenyl)-1,2,3,6-tetrahydropyridine (2.07 g, 10.7 mmol) in acetone (25 mL) was added 1,3-propane sultone (1.41 g, 11.8 mmol). The mixture was stirred at reflux for 2 h. The reaction mixture was cooled to room temperature. The solid was collected by filtration, washed with acetone (2×20 mL) and dried in vacuo. The product was suspended in 50% MeOH/acetone (75 mL). The suspension was stirres at reflux for 5 minutes before 25 mL of cold acetone was added. The solid material was filtered and washed with acetone (2×25 mL). This allowed the isolation of compound J, 1.48 g (44%).

WORKUP

后处理

  1. temperatureat reflux for 2 h
  2. filtrationThe solid was collected by filtration
  3. washwashed with acetone (2×20 mL)
  4. customdried in vacuo
  5. temperatureat reflux for 5 minutes before 25 mL of cold acetone
  6. additionwas added
  7. filtrationThe solid material was filtered
  8. washwashed with acetone (2×25 mL)