HRID1155385

反应详情

EQUATION

反应方程式

HRID 1155385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 50 ml. solution of NaOEt (0.3 g. Na-0.013 mole) was added 2.08 g. (0.013 mole) of diethyl malonate and this was stirred 10 minutes, then stripped to dryness. DMF was added to form a solution and then 1.85 g. (0.0065 mole) of 1-(2-propenyl)7-phenyl-2H-pyrimido[4,5-d][1,3]oxazine-2,4(1H)-dione was added and heated at reflux for 1.5 hours. When cool, the reaction was poured into dilute HCl and the resulting precipitate collected on a filter and rinsed with water. Recrystallization from ethyl acetate gave 1.0 g. of product--m.p. 177°-180° C.

WORKUP

后处理

  1. customto form a solution
  2. temperatureheated
  3. temperatureat reflux for 1.5 hours
  4. temperatureWhen cool
  5. customthe resulting precipitate collected on
  6. filtrationa filter
  7. washrinsed with water
  8. customRecrystallization from ethyl acetate
  9. customgave 1.0 g