HRID712439

反应详情

EQUATION

反应方程式

HRID 712439 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 hexahydro-1H-furo[3,4-c]pyrrole (0.15 g) in acetone (50 mL) was added K2CO3 (0.46 g) and 1-chloro-3-bromopropane (0.42 g, 2.0 eq) in turn. The reaction mixture was heated to reflux for 12 h and filtered. The filtrate was concentrated in vacuo and the residue was dissolved in EtOAc (100 mL). The solution was washed with water twice followed by brine once. The solution was dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was chromatographed with a silica gel column (eluting agent: 20:1 (v/v) EA/CH3OH) to give the title compound (0.13 g, 50.04%). The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 190.7 (M+1).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 12 h
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo
  5. dissolutionthe residue was dissolved in EtOAc (100 mL)
  6. washThe solution was washed with water
  7. dry with materialThe solution was dried over anhydrous Na2SO4
  8. concentrationconcentrated in vacuo
  9. customThe residue was chromatographed with a silica gel column (eluting agent: 20:1 (v/v) EA/CH3OH)