HRID225334
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customto form a solution
- temperatureheated
- temperatureat reflux for 1.5 hours
- temperatureWhen cool
- customthe resulting precipitate collected on
- filtrationa filter
- washrinsed with water
- customRecrystallization from ethyl acetate
- customgave 1.0 g