HRID46161

反应详情

EQUATION

反应方程式

HRID 46161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-(4-bromophenyl)-2,5-dihydro-3H-imidazo[2,1-a]isoindol-5-ol (20.5 g) in AcOH (210 mL) was heated at 125° C. under nitrogen for 6.5 h. The reaction mixture was the cooled to room temperature and concentrated. The resulting residue was partitioned between EtOAc and saturated aqueous NaHCO3 solution. Aqueous layer was extracted with EtOAc (2×). Combined organic layers were washed with brine, dried over Na2SO4 and concentrated. Flash chromatography using a linear gradient of 0-4% MeOH in EtOAc-hexanes (1:1, v/v) afforded title compound as a light yellow solid. Mass. found (M+H)+, 311.0.

WORKUP

后处理

  1. concentrationconcentrated
  2. customThe resulting residue was partitioned between EtOAc and saturated aqueous NaHCO3 solution
  3. extractionAqueous layer was extracted with EtOAc (2×)
  4. washCombined organic layers were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated