HRID2351268

反应详情

EQUATION

反应方程式

HRID 2351268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Hydroxypyrimidine-4,6-dicarboxylic acid (239 mg. 1.30 mmol) was suspended in acetic acid (17M, 60 ml) at 70° with stirring. Zinc dust (600 mg. 9.17 mmol) was added portionwise over a period of 30 min and the mixture was stirred for 1 h at 70° then cooled to room temperature. A solution of oxalic acid (200 mg. 2.22 mmol) in acetic acid (10 ml) was added and the reaction mixture allowed to stand for 5 h. The mixture was filtered and the filtrate evaporated to dryness. The residue was dissolved in hot water (5 ml), filtered and cooled to 4° to 4 days. 2-Oxo-1,2,3,6-tetrahydropyrimidine-4,6-dicarboxylic acid was obtained as off-white crystals (58 mg, 24%).

WORKUP

后处理

  1. stirringthe mixture was stirred for 1 h at 70°
  2. filtrationThe mixture was filtered
  3. customthe filtrate evaporated to dryness
  4. dissolutionThe residue was dissolved in hot water (5 ml)
  5. filtrationfiltered
  6. temperaturecooled to 4° to 4 days