HRID1480812
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
A solution of 6-methyl-2-(methythio)pyrido[3,4-d]pyrimidin-8(7H)-one (Preparation 51, 100 mg, 0.483 mmol) in POCl3 (5 mL) was heated to 70° C. for 1 hour. The reaction mixture was concentrated in vacuo. The residue was partitioned between EtOAc (30 mL) and washed with water (30 mL), dried (MgSO4) and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with 0-20% EtOAc in cyclohexane to give the title compound (28.4 mg, 52%).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- customThe residue was partitioned between EtOAc (30 mL)
- washwashed with water (30 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel column chromatography
- washeluting with 0-20% EtOAc in cyclohexane