HRID473312

反应详情

EQUATION

反应方程式

HRID 473312 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[2-(4-Nitrophenyl)ethyl]{2-[(4-nitrophenyl)oxy]ethyl}amine (253 mg) and 2-(6-bromohexyl)-1H-isoindole-1,3(2H)-dione (1186 mg) were dissolved in DMF (4 ml) and basified by the addition of DIPEA (0.665 ml). The reaction was stirred for 120 h. The reaction mixture was evaporated to dryness and the residue dissolved in DCM, the solution was absorbed onto a pad of silica and purified on a silica cartridge (12 g) eluting with the following gradient: (A=DCM, B=methanol) t=0 min: B=10%; t=7.5 min: B=0%; t=22.5 min: B=5%. The desired product eluted at ˜15% B (isocratically) and evaporation of the solution to dryness gave the title compound (0.364 g).

WORKUP

后处理

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionthe residue dissolved in DCM
  3. customthe solution was absorbed onto a pad of silica
  4. custompurified on a silica cartridge (12 g)
  5. washeluting with the following gradient
  6. customt=0 min
  7. customt=7.5 min
  8. customt=22.5 min
  9. washThe desired product eluted at ˜15% B (isocratically) and
  10. customevaporation of the solution to dryness