HRID1438274

反应详情

EQUATION

反应方程式

HRID 1438274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(4-Bromo-2-ethyl-benzyl)-isoindole-1,3-dione (4 g, 11.7 mmol) and hydrazine (1.8 mL, 58.3 mmol) in chloroform:ethanol (1:1.5, 250 mL) were refluxed for 4 h. The mixture was cooled to room temperature and filtered through a pad of celite. The solution was diluted in water and partitioned. The organic layer was washed with water, saturated sodium bicarbonate, then saturated sodium chloride, dried (Na2SO4), filtered, and then concentrated in vacuo to a yellow oil (2.2 g, 88%). 1H NMR (300 MHz, CDCl3): δ ppm 1.23 (t, J=7.54 Hz, 3H) 1.65 (s, 2H) 2.66 (q, J=7.60 Hz, 2H) 3.84 (s, 2H) 7.19-7.23 (m, 1H) 7.30-7.34 (m, 2H).

WORKUP

后处理

  1. filtrationfiltered through a pad of celite
  2. additionThe solution was diluted in water
  3. custompartitioned
  4. washThe organic layer was washed with water, saturated sodium bicarbonate
  5. dry with materialsaturated sodium chloride, dried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo to a yellow oil (2.2 g, 88%)