HRID1164795

反应详情

EQUATION

反应方程式

HRID 1164795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,4-Dihydro-1-methyl-2(1H)-quinazolinone (2.5 g) is added to a stirred suspension of anhydrous aluminum chloride (10.5 g) in carbon disulfide (120 ml) under nitrogen. 3-Carbomethoxy-2-methyl-propionyl chloride (2.5 g) is added dropwise to the stirred suspension, which is refluxed for about 18 hours and cooled to RT. The liquid phase is decanted and the residue treated with ice/H2O and 6N HCl (25 ml). The aqueous mixture is extracted with methylene chloride, the organic extract dried, filtered and concentrated in vacuo, affording the desired product as an oil which is used in the next step without further purification.

WORKUP

后处理

  1. temperatureis refluxed for about 18 hours
  2. customThe liquid phase is decanted
  3. additionthe residue treated with ice/H2O and 6N HCl (25 ml)
  4. extractionThe aqueous mixture is extracted with methylene chloride
  5. extractionthe organic extract
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo