HRID2200890

反应详情

EQUATION

反应方程式

HRID 2200890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In DCM (30 mL) were dissolved 4-((3-chloro-4-methoxybenzyl)amino)-2-(methylsulfinyl)-N-(pyrimidin-2-ylmethyl)pyrimidine-5-formamide (429 mg, 0.96 mmol) and DIEA (0.22 mL, 1.12 mmol). 2-Methyl-2,7-diazaspiro[4.4]nonane (154 mg, 1.1 mmol) was then added. The reaction was conducted at ambient temperature overnight. The solvent was removed by rotary evaporation, followed by addition of water and extraction with ethyl acetate. The organic phase was dried over sodium sulfate and purified by silica gel column chromatography (DCM/methanol=20/1 to 10/1) to give a white solid (20 mg, 4% yield).

WORKUP

后处理

  1. customThe solvent was removed by rotary evaporation
  2. additionfollowed by addition of water and extraction with ethyl acetate
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. custompurified by silica gel column chromatography (DCM/methanol=20/1 to 10/1)