HRID442859

反应详情

EQUATION

反应方程式

HRID 442859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of Compound 88 (1.0 g, 1.98 mmol) obtained in Example 88 in 10 ml of N,N-dimethylformamide was portionwise added sodium hydride (60% in oil, 166 mg, 4.15 mmol) with stirring at room temperature, and 2-dimethylaminoethylchloride hydrochloride (298 mg, 2.07 mmol) was added thereto, followed by heating to 80° C. and then stirring for one hour. A saturated aqueous solution of ammonium chloride was added to the reaction solution for neutralization, water was added thereto, and the resulting crystals were collected by filtration to give 1.1 g of a crude product. The obtained crude product was recrystallized from ethanol (65 ml) to give 0.67 g (yield: 59%) of the title compound.

WORKUP

后处理

  1. temperatureby heating to 80° C.
  2. stirringstirring for one hour
  3. additionwas added
  4. filtrationthe resulting crystals were collected by filtration
  5. customto give 1.1 g of a crude product
  6. customThe obtained crude product
  7. customwas recrystallized from ethanol (65 ml)