HRID860078

反应详情

EQUATION

反应方程式

HRID 860078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 2,6-dichloro-4-aminopyrimidine 18-1 (Avocado; 4.8 g, 29.3 mmol), ethylamine hydrochloride (7.0 g, 85.8 mmol), Et3N (20 mL, 144 mmol) and n-butanol (150 mL) was heated to 90° C. for 6 hours. After cooling, the solvent was removed in vacuo and the residue partitioned between saturated Na2CO3 solution and EtOAc. The EtOAc layer was washed with brine, dried (MgSO4) and concentrated to give an orange solid. Purification by column chromatography (EtOAc/hexane 1:1) gave the title compound 18-2 as a white solid.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe solvent was removed in vacuo
  3. customthe residue partitioned between saturated Na2CO3 solution and EtOAc
  4. washThe EtOAc layer was washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customto give an orange solid
  8. customPurification by column chromatography (EtOAc/hexane 1:1)