HRID1984624
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
PROCEDURE
实验过程
The solution of 7-hydroxy-6-phenylpyrido[2,3-d]pyrimidine-2-carbonitrile (0.300 g, 1.21 mmol) in CH3CN and POCl3 (2 mL) was heated to 100° C. for 4 h. The mixture was concentrated and the residue was basified with saturated NaHCO3 at 0° C. Extracted with CH2Cl2 and the combined organic layer was dried, filtered and concentrated. The residue was purified by silica gel chromatography (10-20% EtOAc in hexane) to give the title compound. LRMS m/z (M+H) Calcd: 267.7, found: 267.2.
WORKUP
后处理
- concentrationThe mixture was concentrated
- customwas basified with saturated NaHCO3 at 0° C
- extractionExtracted with CH2Cl2
- customthe combined organic layer was dried
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by silica gel chromatography (10-20% EtOAc in hexane)