HRID492637

反应详情

EQUATION

反应方程式

HRID 492637 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 2-Benzyl-5-methoxy-2,3-dihydro-1H-isoindol (580.0 mg, 2.42 mmol) and 48% HBr (aq) (20 mL). Reflux the reaction for 5 hours and then cool to room temperature. Concentrate the reaction mixture under reduced pressure then add to 5 g a SCX column. Wash the column with MeOH and elute with 1N NH3-MeOH to afford 265.4 mg, 1.17 mmol (49% yield) of the title compound as a brown solid: 1H NMR (500 MHz, d-Methanol); 3.8-3.9 (4H, m), 3.91 (2H, s), 6.6-6.7 (2H, m), 7.0 (1H, d), 7.2-7.5 (4H, m); MS m/z 226 (M+1).

WORKUP

后处理

  1. temperatureReflux
  2. customthe reaction for 5 hours
  3. concentrationConcentrate the reaction mixture under reduced pressure
  4. additionthen add to 5 g a SCX column
  5. washWash the column with MeOH
  6. washelute with 1N NH3-MeOH