HRID1155391

反应详情

EQUATION

反应方程式

HRID 1155391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of sodium ethoxide (0.9 g. .039 g. atom of sodium in 75 ml. of ethanol) was added 6.24 g. (0.03 mole) of diethyl malonate. The ethanol was removed in a rotary evaporator. To the residue was added 100 ml. of dimethyl formamide followed by 3.3 g. (0.013 mole) of 7-methylthio-1-isopropyl-2H-pyrimido[4,5-d][1,3]oxazine-2,4(1H)-dione. The reaction mixture was heated under reflux for 1 hour, cooled in ice and poured into 400 ml. of water. The solution was acidified with conc. hydrochloric acid and the resulting product was collected by suction filtration. Recrystallization from ethanol gave 2 g. of product--m.p. 138°-140° C.

WORKUP

后处理

  1. customThe ethanol was removed in a rotary evaporator
  2. additionTo the residue was added 100 ml
  3. temperatureThe reaction mixture was heated
  4. temperatureunder reflux for 1 hour
  5. temperaturecooled in ice
  6. additionpoured into 400 ml
  7. filtrationthe resulting product was collected by suction filtration
  8. customRecrystallization from ethanol
  9. customgave 2 g