HRID354893

反应详情

EQUATION

反应方程式

HRID 354893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of methyl 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (5.42 g) and anhydrous lithium iodide (13.55 g) in dry pyridine (54 ml) was stirred at 100° C. for 1.5 hours. The reaction mixture was cooled to give crytals which were collected by filtration and washed with pyridine. The crystals were suspended in water (200 ml). The suspension was adjusted to pH 2.5-3.0 with conc. hydrochloric acid to give yellow crystals, which were separated by filtration, washed with water and dried. The crude crystals were washed with a mixture of chloroform and methanol (1:1) two times and dried. There was obtained crystalline 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylic acid (3.80 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customto give crytals which
  3. filtrationwere collected by filtration
  4. washwashed with pyridine
  5. customto give yellow crystals, which
  6. customwere separated by filtration
  7. washwashed with water
  8. customdried
  9. washThe crude crystals were washed with a mixture of chloroform and methanol (1:1) two times
  10. customdried