HRID276864

反应详情

EQUATION

反应方程式

HRID 276864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 2.0 g of 4-chloro-6-fluoro-[1.7]naphthyridine-3-carbonitrile in 50 mL of methanol was added 1.9 g of 2,4-dichloroaniline. After refluxing the reaction under an inert atmosphere for 2 hours, the reaction mixture was poured into a mixture of brine and saturated aqueous sodium bicarbonate and the resultant crystals were filtered and washed with water. The product was then recrystallized from chloroform/hexanes. Drying in vacuo yielded 2.6 g (80%) of 4-(2,4-dichloro-phenylamino)-6-fluoro-[1.7]naphthyridine-3-carbonitrile as yellow needles: melting point 206-208° C.; mass spectrum (m/e): M+H 332.8.

WORKUP

后处理

  1. temperatureAfter refluxing
  2. customthe reaction under an inert atmosphere for 2 hours
  3. filtrationthe resultant crystals were filtered
  4. washwashed with water
  5. customThe product was then recrystallized from chloroform/hexanes
  6. customDrying in vacuo