HRID49797

反应详情

EQUATION

反应方程式

HRID 49797 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-bromo-2-chloro-4-(4-methoxyphenoxy)pyrimidine (Method 1, 200 mg, 0.63 mmol) and 4-[2-hydroxy-3-(N,N-dimethylamino)propoxy]aniline hydrochloride (Method 8, 156 mg, 0.56 mmol) in NMP (4 ml) was heated at 100° C. for 6 hours. Silica (1 g) was added and volatile material was removed by evaporation. The residue was purified by column chromatography, eluting with 0-10% 2.0M methanolic ammonia solution in DCM, to give the product as a colourless solid (173 mg, 56%). MS (MH+): 489, 491; HPLC (RT): 4.68.

WORKUP

后处理

  1. additionSilica (1 g) was added
  2. customvolatile material was removed by evaporation
  3. customThe residue was purified by column chromatography
  4. washeluting with 0-10% 2.0M methanolic ammonia solution in DCM