HRID1719964

反应详情

EQUATION

反应方程式

HRID 1719964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of methyl 4-oxo-10-(3-cyclopentylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (5.72 g) and anhydrous lithium iodide (14.3 g) in dry pyridine (59 ml) was stirred at 120° C. for 1.5 hours. The reaction mixture was concentrated under reduced pressure to give a crystalline residue, which was suspended in water (100 ml). The suspension was adjusted to pH 1.7 with conc. hydrochloric acid to yield yellow crystals, which were separated by filtration, washed with water and dried. Recrystallization from N,N-dimethylformamide gave crystalline 4-oxo-10-(3-cyclopentylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylic acid (4.4 g).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customto give a crystalline residue, which
  3. customto yield yellow crystals, which
  4. customwere separated by filtration
  5. washwashed with water
  6. customdried
  7. customRecrystallization from N,N-dimethylformamide