HRID225331

反应详情

EQUATION

反应方程式

HRID 225331 的结构方程式

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

  1. customevaporated to dryness
  2. additionDMF was added until a solution
  3. temperaturethis mixture refluxed 2 hours
  4. customThe chilled reaction
  5. filtrationthe ensuing precipitate filtered off
  6. washrinsed with water
  7. customRecrystallization from ethyl acetate
  8. customgave 3.5 g