HRID920290

反应详情

EQUATION

反应方程式

HRID 920290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a solution of 4-(4-Chloro-3-(trifluoromethyl)phenoxy)benzaldehyde (13 g, 43.2 mmol) and ammonium acetate (1.67 g, 21.62 mmol) in HOAc (40 mL), was added nitromethane (6.99 mL, 130 mmol). The reaction mixture was stirred at 120° C. for 5 h, and concentrated. The residue was dissolved in DCM (150 mL), washed with sat. aqueous NaHCO3 (100 mL×2), brine and then, dried over anhydrous Na2SO4 and concentrated to afford the title compound as a brown solid (14.3 g, 63% yield).

WORKUP

后处理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in DCM (150 mL)
  3. washwashed with sat. aqueous NaHCO3 (100 mL×2), brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated