HRID1930543

反应详情

EQUATION

反应方程式

HRID 1930543 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
76 °C

PROCEDURE

实验过程

Hydrochloric acid (2M aq, 2 ml) was added to a solution of tert-butyl 4-(benzylamino)-2-(4-(oxazol-5-yl)phenylamino)-7,8-dihydropyrido[4,3-d]pyrimidine-6(5H)-carboxylate (0.15 g, 0.30 mmol, Example 6a) in MeOH (4 mL). The reaction was heated in an open reaction vessel to 76° C. for 1 h and the product precipitated out from the solution as it was cooled. The crude product was filtered off and washed with water. The crude salt was dissolved in water and precipitated when saturated NaHCO3 was added. The product was filtered off and purified by preparative HPLC to give N4-benzyl-N2-(4-(oxazol-5-yl)phenyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine-2,4-diamine (0.090 g, 75%). MS (ESI+)/(ESI−) m/z 399/397

WORKUP

后处理

  1. customthe product precipitated out from the solution as it
  2. temperaturewas cooled
  3. filtrationThe crude product was filtered off
  4. washwashed with water
  5. dissolutionThe crude salt was dissolved in water
  6. customprecipitated when saturated NaHCO3
  7. additionwas added
  8. filtrationThe product was filtered off
  9. custompurified by preparative HPLC