HRID1434513

反应详情

EQUATION

反应方程式

HRID 1434513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chloro-4-morpholino-6-nitro-pyrido[2,3-d]pyrimidine (4.4 g; 15 mmol) was dissolved in tetrahydrofuran (100 mL). To the solution was added morpholino-2-ethanol (2.4 g; 18 mmol), and it was chilled in a dry ice bath. Sodium 400 mg; 18 mmol). was then added, and it was allowed to warm to room temperature and stirred overnight. The solvent was then evaporated, and the solid was dissolved in dichloromethane (50 mL), washed with water (3×10 mL), dried over magnesium sulfate, and purified by column chromatography to give 4-morpholin-4-yl-2-(2-morpholin-4-yl-ethoxy)-6-nitro-pyrido[2,3-d]pyrimidine (3.35 g).

WORKUP

后处理

  1. temperaturewas chilled in a dry ice bath
  2. additionwas then added
  3. customThe solvent was then evaporated
  4. dissolutionthe solid was dissolved in dichloromethane (50 mL)
  5. washwashed with water (3×10 mL)
  6. dry with materialdried over magnesium sulfate
  7. custompurified by column chromatography