HRID2067746
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
3-Benzyl-5-hydroxy-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (5.5 g, 18.5 mmol) was dissolved in excess POCl3 (50 mL) and heated at reflux for 1 hour. POCl3 was removed in vacuo and the residue dissolved in DCM then quickly washed with saturated sodium bicarbonate solution until neutral pH was observed. The organic layer was dried over MgSO4 and evaporated to dryness to give 7.3 g of the title compound as an impure reddish brown solid. [M+H] calc'd for C16H14ClN3O2, 315; found, 315.
WORKUP
后处理
- temperatureheated
- temperatureat reflux for 1 hour
- customPOCl3 was removed in vacuo
- dissolutionthe residue dissolved in DCM
- washthen quickly washed with saturated sodium bicarbonate solution until neutral pH
- dry with materialThe organic layer was dried over MgSO4
- customevaporated to dryness