反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe product precipitated out from the solution as it
- temperaturewas cooled
- filtrationThe crude product was filtered off
- washwashed with water
- dissolutionThe crude salt was dissolved in water
- customprecipitated when saturated NaHCO3
- additionwas added
- filtrationThe product was filtered off
- custompurified by preparative HPLC