HRID971462

反应详情

EQUATION

反应方程式

HRID 971462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 125 g (0.458 mole) of 6-chloro-4-phenyl-2(1H)quinazolinone 3-oxide, 3,250 ml of N,N-dimethylformamide and 75 g of powdered anhydrous potassium carbonate was heated to 50°. After heating for approximately 30 minutes at this temperature, an increased solubility of the suspended solid due to formation of the potassium salt of I was observed. At this point, 150 g (65.8 ml) of methyl iodide was added dropwise at a fast rate. The reaction with the methyl iodide was somewhat exothermic and caused the pot temperature to rise to 58°. Stirring at 50°-55° was continued for 1 hour. The contents of the flask were cooled and filtered and the solid obtained was thoroughly washed with water. The product, 6-chloro-1-methyl-4-phenyl-2(1H)quinazolinone 3-oxide was obtained in 80% yield (103.2 g), mp 253.5°-254°.

WORKUP

后处理

  1. temperaturewas heated to 50°
  2. temperatureAfter heating for approximately 30 minutes at this temperature
  3. customto rise to 58°
  4. temperatureThe contents of the flask were cooled
  5. filtrationfiltered
  6. customthe solid obtained
  7. washwas thoroughly washed with water