HRID127375
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
50 ml. of NaOEt (0.5 g. Na -0.021 mole) was added to 3.4 g. (0.021 mole) of ethyl malonate and stirred 10 minutes, then evaporated to dryness. DMF was added until a solution was achieved and then 3.2 g. (0.011 mole) of 1-(2-methoxyethyl)-7-phenyl-2H-pyrimido[4,5-d][1,3]oxazine-2,4(1H)-dione was added and this mixture refluxed 2 hours. The chilled reaction was poured into dilute HCl and the ensuing precipitate filtered off and rinsed with water. Recrystallization from ethyl acetate gave 3.5 g. of the title product--m.p. 178°-179° C.
WORKUP
后处理
- customevaporated to dryness
- additionDMF was added until a solution
- temperaturethis mixture refluxed 2 hours
- customThe chilled reaction
- filtrationthe ensuing precipitate filtered off
- washrinsed with water
- customRecrystallization from ethyl acetate
- customgave 3.5 g