HRID707677

反应详情

EQUATION

反应方程式

HRID 707677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Toluene-4-thiosulfonic acid S-(3-chloro-propyl) ester (4.9 g, 18.4 mol, 1.00 eq.), N-methylpiperazine (1.9 g, 19.3 mmol) 1.05 eq.) and potassium carbonate (2.7 g, 19.4 mmol, 1.05 eq.) were stirred together in acetonitrile (100 mL) at room temperature for 64 hours. The mixture was concentrated and the residue was partitioned between ethyl acetate (500 ml) and water (250 ml). The organic solution was washed with water (2×200 mL), dried using MgSO4, concentrated and purified by MPLC to give a light yellow oil weighing 2.1 g (36%).

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. customthe residue was partitioned between ethyl acetate (500 ml) and water (250 ml)
  3. washThe organic solution was washed with water (2×200 mL)
  4. customdried
  5. concentrationconcentrated
  6. custompurified by MPLC
  7. customto give a light yellow oil