HRID746254

反应详情

EQUATION

反应方程式

HRID 746254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7 g of 6-chloro-3-propyluracil, 10.28 g of butyl bromide, 10.28 g of potassium carbonate, 6 g of potassium iodide and 80 ml of dimethylformamide was stirred at room temperature for 23 hours. After the reaction solution was concentrated to dryness under reduced pressure, 300 ml each of chloroform and water were added to the residue, and the mixture was shaken. The chloroform layer was washed with water and then concentrated to dryness under reduced pressure to give 6-chloro-1-butyl-3-propyluracil as a brown oily substance. This product, without being purified, was dissolved in 20 ml of ethanol, and 20 ml of 100% hydrazine hydrate was added to the solution, followed by stirring at room temperature for 1 hour. The reaction solution was concentrated to dryness under reduced pressure and the residue was washed with water and recrystallized from a mixture of ethanol, ethyl acetate and isopropyl ether to give 7 g of yellow prisms of 6-hydrazino-1-butyl-3-propyluracil melting at 146°-147° C.

WORKUP

后处理

  1. concentrationAfter the reaction solution was concentrated to dryness under reduced pressure, 300 ml each of chloroform and water
  2. additionwere added to the residue
  3. stirringthe mixture was shaken
  4. washThe chloroform layer was washed with water
  5. concentrationconcentrated to dryness under reduced pressure