HRID1266294

反应详情

EQUATION

反应方程式

HRID 1266294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 3.5 g of 4-chloro-6-fluoro-[1,7]naphthyridine-3-carbonitrile in 100 mL of absolute ethanol was added 2.3 mL of 4-chloro-2-fluoroaniline. After stirring the reaction under an inert atmosphere for 24 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/ethyl acetate/hexanes. Drying in vacuo yielded 1.9 (40%) of 4-(4-chloro-2-fluoro-phenylamino)-6-fluoro-[1,7]naphthyridine-3-carbonitrile as yellow needles: melting point 249-252° C.; mass spectrum (m/e): M+H 316.9.

WORKUP

后处理

  1. customthe reaction under an inert atmosphere for 24 hours
  2. filtrationthe resultant crystals were filtered
  3. washwashed with water
  4. customThe product was then recrystallized from chloroform/ethyl acetate/hexanes
  5. customDrying in vacuo