HRID364624

反应详情

EQUATION

反应方程式

HRID 364624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 5.8 g (0.03 mole) 2-mercapto-3-allyl-4(3H)-quinazolinone (the product of Example 5) in 200 ml dimethoxyethane, 5.4 g (0.05 mole) chloromethyl thiocyanate and 2.4 g (0.05 mole) 50% sodium hydride were added. The resulting mixture was stirred overnight at ambient temperature, refluxed at 50° C. for 8 hours, stirred overnight, refluxed at 50° C. for 8 hours and stirred overnight. The reaction mixture was washed with water, extracted with methylene chloride, dried over magnesium sulfate and stripped. The oily residue was triturated with ether, to give the above-identified product, as a solid, melting point 73°-76° C.

WORKUP

后处理

  1. temperaturerefluxed at 50° C. for 8 hours
  2. stirringstirred overnight
  3. temperaturerefluxed at 50° C. for 8 hours
  4. stirringstirred overnight
  5. washThe reaction mixture was washed with water
  6. extractionextracted with methylene chloride
  7. dry with materialdried over magnesium sulfate
  8. customThe oily residue was triturated with ether
  9. customto give the above-identified product