HRID598074

反应详情

EQUATION

反应方程式

HRID 598074 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-dipropylamino-5-methoxy-3-methylquinazolin-4(3H)-one (130 mg, 0.449 mmol) in dichloroethane (2 ml) was added boron tribromide-methyl sulfide complex (1M solution in dichloromethane, 0.899 ml, 0.899 mmol) under nitrogen atmosphere. The mixture was refluxed for 2 h. The reaction was quenched with water and stirred for 10 min at room temperature. The aqueous phase was extracted with ether. The extract was washed with brine, dried over magnesium sulfate and concentrated under vacuum to afford 123 mg (99%) of the title compound. The residue was used for the next reaction without further purification.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 h
  2. customThe reaction was quenched with water
  3. extractionThe aqueous phase was extracted with ether
  4. washThe extract was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vacuum