HRID2408997

反应详情

EQUATION

反应方程式

HRID 2408997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(4-chlorophenyl)-6,7-dimethoxyquinazolin-4(3H)-one (200 mg), thionyl chloride (10 mL) and DMF (0.3 mL) was refluxed for 2 h. Solvents were removed under vacuum. The mixture was poured into ice cold water and stirred for 10 min. The solution was basified with ammonia and stirred for 5 min. The solution was extracted with chloroform (3×100 mL) and the combined chloroform layer was washed with water, brine and dried over sodium sulfate. The solution was filtered and evaporated the solvent to give the product as an yellow color solid (180 mg, 86%), mp 204-206° C. 1H NMR (400 MHz, DMSO-d6): δ 8.47 (2H, d, J=8.4 Hz), 7.66 (2H, d, J=8.4 Hz), 7.52 (1H, s), 7.44 (1H, s), 4.08 (3H, s), 4.05 (3H, s).

WORKUP

后处理

  1. temperaturewas refluxed for 2 h
  2. customSolvents were removed under vacuum
  3. additionThe mixture was poured into ice cold water
  4. stirringstirred for 5 min
  5. extractionThe solution was extracted with chloroform (3×100 mL)
  6. washthe combined chloroform layer was washed with water, brine
  7. dry with materialdried over sodium sulfate
  8. filtrationThe solution was filtered
  9. customevaporated the solvent