HRID918241

反应详情

EQUATION

反应方程式

HRID 918241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 250 ml Erlenmeyer flask equipped with a magnetic stirrer and oil bath for heating was charged with 8.0 g (0.07 mole) of p-aminophenol and 25 ml of dimethylformamide. After the p-aminophenol was dissolved by stirring, 9.05 g (0.03 mole) of 2-[2-(5-nitro-2-furyl)vinyl]-4-chloroquinazoline (IV) was added. The reaction mixture was then heated at 70°-90°C for 2 hours after which 60 ml of water was added and the solution after cooling was placed in a refrigerator for crystallization. After three days, the brown yellow solid was collected, washed first with water, then methanol and then dried to obtain 7.20 g of product melting at 250°-60°C with decomposition. Recrystallization from a 1:1 dimethylformamidemethanol mixture gave 6.5 g of orange crystals of the purified product which melted at 270°-2°C with decomposition.

WORKUP

后处理

  1. customA 250 ml Erlenmeyer flask equipped with a magnetic stirrer and oil bath
  2. temperaturefor heating
  3. additionwas added
  4. temperaturethe solution after cooling
  5. customwas placed in a refrigerator for crystallization
  6. customthe brown yellow solid was collected
  7. washwashed first with water
  8. dry with materialmethanol and then dried