HRID1768562

反应详情

EQUATION

反应方程式

HRID 1768562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product of Step D (17 g, 86 mole), 4,5-dichloro-6-ethylpyrimidine (15 g, 86 mole) and triethylamine (24 mL, 170 mole) were dissolved in toluene (65 mL). The reaction mixture was heated to reflux overnight and then cooled. Ether and water were added and the mixture was partitioned. The aqueous phase was extracted two times with ether and the combined organic phases were dried (MgSO4) and concentrated. The resultant solid was recrystallized from acetonitrile to give the title compound as a white solid (17 g, 60% yield), mp 79°-80° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux overnight
  3. temperaturecooled
  4. customthe mixture was partitioned
  5. extractionThe aqueous phase was extracted two times with ether
  6. dry with materialthe combined organic phases were dried (MgSO4)
  7. concentrationconcentrated
  8. customThe resultant solid was recrystallized from acetonitrile