HRID1972392

反应详情

EQUATION

反应方程式

HRID 1972392 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A 100 mL round-bottomed flask was charged with 2-((tetrahydro-2H-pyran-4-yl)methyl)piperazine (0.950 g, 5.16 mmol), 20 mL of CH2Cl2, triethylamine (0.790 mL, 5.67 mmol), and 2-thiophenesulfonyl chloride (0.942 mL, 5.16 mmol, Sigma-Aldrich, St. Louis, Mo.). After 15 min at room temperature, the mixture was diluted with water (50 mL) and CH2Cl2 (50 mL), the organics were separated, dried (MgSO4) and concentrated to give a dark oil. To this oil was added 50 mL of ether and 10 mL of 1N HCl in ether. The resulting white precipitate was collected by filtration to give 3-(tetrahydro-2H-pyran-4-ylmethyl)-1-(2-thiophenylsulfonyl)piperazine hydrochloride (1.45 g) as an orange solid.

WORKUP

后处理

  1. customthe organics were separated
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customto give a dark oil
  5. filtrationThe resulting white precipitate was collected by filtration