HRID868148

反应详情

EQUATION

反应方程式

HRID 868148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 1,4-dihydro-6,7-dimethoxy-4-oxo-N-(2-oxo-1-imidazolidinyl)-3-quinolinecarboxamide (23.1 g, 69.5 mmol) in 1.2 l of dichloromethane, a solution of boron tribromide (104.5 g, 417 mmol) was added dropwise at 0° C. After stirring for 3 days at room temperature, the precipitate was filtered off, washed with dichloromethane and was then added to 300 ml of methanol under ice cooling. After stirring for 2 hours, the solid was filtered off, washed with methanol and dried in vacuo. Yield: 24.8 g (still contained some starting material). The reaction was repeated to give 18.4 g of the title compound after methanol treatment, melting point>300° C.

WORKUP

后处理

  1. filtrationthe precipitate was filtered off
  2. washwashed with dichloromethane
  3. additionwas then added to 300 ml of methanol under ice cooling
  4. stirringAfter stirring for 2 hours
  5. filtrationthe solid was filtered off
  6. washwashed with methanol
  7. customdried in vacuo