HRID2223369

反应详情

EQUATION

反应方程式

HRID 2223369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A suspension of 2H-naphth[2,3-d][1,3]oxazine-2,4(1H)-dione (216 mg) and 2-amino-5-chloropyridine (202 mg) in xylene (5 ml) is stirred at 150° C. for 13 hours, and thereto added 4-dimethylaminopyridine (14.4 mg) and the mixture is stirred at 150° C. for another 3 hours. The reaction solution is concentrated under reduced pressure and the resulting residue is suspended in ethyl acetate, and filtered to remove insoluble materials. The filtrate is concentrated under reduced pressure, and the residue is purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=2/1) to give 3-amino-N-(5-chloropyridin-2-yl)-2-naphthamide (24 mg).

WORKUP

后处理

  1. concentrationThe reaction solution is concentrated under reduced pressure
  2. filtrationfiltered
  3. customto remove insoluble materials
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. customthe residue is purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=2/1)