HRID415518

反应详情

EQUATION

反应方程式

HRID 415518 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-chloro[1,5]naphthyridin-3-amine (2.0 g, 11 mmol) and 4-chlorobutyryl chloride (4.7 g, 33 mmol) in 1,2-dichloroethane (75 mL) was heated at reflux for 20 hours. The reaction mixture was then concentrated under reduced pressure and the residue washed with two 25 mL portions of hexane. The solid was then taken up in methanol (35 mL), 1.0 mL of 10% solution of sodium hydroxide in water was added, and the solution was stirred at room temperature for 4 hours. The reaction mixture was then concentrated under reduced pressure to provide 4-chloro-N-(4-chloro[1,5]naphthyridin-3-yl)butanamide which was used directly in the next step without further purification.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 20 hours
  3. concentrationThe reaction mixture was then concentrated under reduced pressure
  4. washthe residue washed with two 25 mL portions of hexane
  5. addition1.0 mL of 10% solution of sodium hydroxide in water was added
  6. concentrationThe reaction mixture was then concentrated under reduced pressure