HRID61533

反应详情

EQUATION

反应方程式

HRID 61533 的结构方程式

PROCEDURE

实验过程

To a suspension of 2-(3-nitrophenyl)quinazolin-4(3H)-one (5.7 g, 21.32 mmole) in thionyl chloride (70 mL) was added of DMF (2 mL). The reaction mixture was refluxed for 4.5 h. The reaction was then concentrated in vacuo and residue suspended in a mixture of CH2Cl2 (400 mL) and CHCl3 (500 mL). The organic layer was washed with water, saturated NaHCO3, water, brine, dried with Na2SO4 and concentrated in vacuo. The residue was dried under high vacuum to afford 4-chloro-2-(3-nitrophenyl)quinazoline as an off-white solid. (6.0 g, mmol, 97%).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 4.5 h
  2. concentrationThe reaction was then concentrated in vacuo and residue
  3. additionsuspended in a mixture of CH2Cl2 (400 mL) and CHCl3 (500 mL)
  4. washThe organic layer was washed with water, saturated NaHCO3, water, brine
  5. dry with materialdried with Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was dried under high vacuum