HRID2241394

反应详情

EQUATION

反应方程式

HRID 2241394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A 250 mL round-bottomed flask was charged with 2-(3-fluoro-4-methoxyphenylamino)-N-(4-fluorophenyl)nicotinamide (8.00 g, 22.5 mmol) and DCM (75 mL). The reaction mixture was cooled to 0° C. and BBr3 (10.9 ml, 115 mmol) was added dropwise over 5 minutes. The reaction mixture was stirred for 2 hours, then slowly quenched by pipetting the reaction into a flask (500 mL) containing saturated NaHCO3 (20 mL), water (150 mL). This solution was extracted with EtOAc. The organic layer was dried and concentrated to provide the product 6.25 g (73%). LRMS M−1 (339.9) observed.

WORKUP

后处理

  1. customslowly quenched
  2. customthe reaction into a flask (500 mL)
  3. extractionThis solution was extracted with EtOAc
  4. customThe organic layer was dried
  5. concentrationconcentrated