HRID1817792

反应详情

EQUATION

反应方程式

HRID 1817792 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

1-Propyl, 3-cyclopropyl, 6-aminouracil (2) (12.8 g, 61.2 mmol ) was dissolved in acetic acid (25 ml) in 200 ml of water and the mixture was cooled to 10° C. To the uracil solution, NaNO2 (7.6 g, 110.1 mmol ) in 50 ml of water was added dropwise at 10° C. The mixture was stirred at 10° C. for 30 min and then at room temperature for 1 h. The solvent was removed under reduced pressure and the residue was dissolved in the mixture of absolute ethanol and CH2Cl2 (1:1) and boiled for 20 min. The hot mixture was filtered through a layer of Celite 545 to remove the insoluble inorganic salts. The mother liquid was evaporated under reduced pressured to remove the solvent to give 1-propyl, 3-cyclopropyl, 6-amino, 5-nitrosouracil (4) (11.4 g, 78%).

WORKUP

后处理

  1. waitat room temperature for 1 h
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in the mixture of absolute ethanol and CH2Cl2 (1:1)
  4. waitboiled for 20 min
  5. filtrationThe hot mixture was filtered through a layer of Celite 545
  6. customto remove the insoluble inorganic salts
  7. customThe mother liquid was evaporated
  8. customto remove the solvent