HRID2200891

反应详情

EQUATION

反应方程式

HRID 2200891 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In THF (10 mL) were dissolved 4-((3-chloro-4-methoxybenzyl)amino)-2-(methyl sulfinyl)-N-(pyrimidin-2-ylmethyl)pyrimidine-5-formamide (152 mg, 0.34 mmol) and 2-methyl-2,7-diazaspiro[3.5]nonane (70 mg, 0.50 mmol). Then triethylamine (68 mg, 0.67 mmol) was added dropwisely. The reaction was conducted at ambient temperature for 4 h. The solvent was removed by rotary evaporation, followed by addition of water and extraction with DCM. The organic phase was dried over sodium sulfate and purified by silica gel column chromatography (DCM/methanol=20/1) to give 4-((3-chloro-4-methoxybenzyl)amino)-2-(7-methyl-2,7-diazaspiro[3.5]nonan-2-yl)-N-(pyrimidin-2-ylmethyl)pyrimidine-5-formamide as a white solid (16 mg, 9% yield).

WORKUP

后处理

  1. customThe solvent was removed by rotary evaporation
  2. additionfollowed by addition of water and extraction with DCM
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. custompurified by silica gel column chromatography (DCM/methanol=20/1)