HRID1509951

反应详情

EQUATION

反应方程式

HRID 1509951 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Cytosine (3.0 g, 27 mmol) and dimethyl-formamide-dimethylacetal (40 mL) was added to 100 mL mad apple-type flask with a magnetic stirrer, heated at 120° C. with constant stirring. Then, trifluoroacetic acid (0.2 mL) was added and the mixture was allowed to stir for 18 hr. The reacting solution was cooled to room temperature, followed by cooling in ice bath. The white precipitation was filtrated, dissolved in dichloromethane and ethanol, and changed to powders by hexane. The solids were collected and dried under vacuum. Thus, 4-N—(N,N-dimethylaminomethylene)-1-methylcytosine was obtained as white solids (3.6 g, yield, 74%). 1H-NMR (400 MHz, DMSO-d6)

WORKUP

后处理

  1. temperatureThe reacting solution was cooled to room temperature
  2. temperatureby cooling in ice bath
  3. customThe white precipitation
  4. filtrationwas filtrated
  5. dissolutiondissolved in dichloromethane
  6. customThe solids were collected
  7. customdried under vacuum