HRID1804632

反应详情

EQUATION

反应方程式

HRID 1804632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1.0 g (4.2 mmol) of the title compound from Step B in 30 ml toluene was added 2.9 g (9.2 mmol) of 21% sodium ethoxide. The reaction was refluxed overnight. After cooling down to RT, the reaction was filtered and the solid was collected. The solid was then dissolved in 20 ml water, and acidified by acetic acid. The solid was filtered and washed with dichloromethane and dried. The solid was added to 30 ml of 10% HCl aqueous solution and refluxed for 3 hr. Then HCl was evaporated to give 350 mg (62% yield) of the title compound. LC/MS: (M+1) 136.1

WORKUP

后处理

  1. temperatureThe reaction was refluxed overnight
  2. filtrationthe reaction was filtered
  3. customthe solid was collected
  4. dissolutionThe solid was then dissolved in 20 ml water
  5. filtrationThe solid was filtered
  6. washwashed with dichloromethane
  7. customdried
  8. additionThe solid was added to 30 ml of 10% HCl aqueous solution
  9. temperaturerefluxed for 3 hr
  10. customThen HCl was evaporated