HRID442859
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureby heating to 80° C.
- stirringstirring for one hour
- additionwas added
- filtrationthe resulting crystals were collected by filtration
- customto give 1.1 g of a crude product
- customThe obtained crude product
- customwas recrystallized from ethanol (65 ml)