HRID707676

反应详情

EQUATION

反应方程式

HRID 707676 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 (12.0 g, 45.3 mol, 1.00 eq.), N-ethylisopropylamine (4.2 g, 48.0 mmol, 1.05 eq.) and potassium carbonate (6.9 g, 49.9 mmol, 1.10 eq.) were stirred together in acetonitrile (160 mL) at 60° C. for 18 hours. The mixture was concentrated in vacuo and the residue was partitioned between ethyl acetate (500 mL) and water (250 mL). The organic solution was washed with brine (250 mL), dried (MgSO4) and the resulting oil was purified by MPLC chromatography to give an oil weighing 2.98 g (21%).

WORKUP

后处理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was partitioned between ethyl acetate (500 mL) and water (250 mL)
  3. washThe organic solution was washed with brine (250 mL)
  4. dry with materialdried (MgSO4)
  5. customthe resulting oil was purified by MPLC chromatography
  6. customto give an oil