HRID2376717
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 3-(dimethylamino)-1-(4-fluorophenyl)-2-(4-pyridyl)prop-2-en-1-one (12.77 g, 47.2 mmol, obtained in reference example 7) in DMF (175 mL), 2-cyanoacetamide (4.41 g, 52.0 mmol) was added under argon atmosphere. Then, sodium methoxide (5.35 g, 99.2 mmol) was added and heated to reflux for 1 hour. The mixture was allowed to cool, concentrated and diluted with water. The pH was adjusted to 4 with 1 N HCl. A precipitate was obtained that was filtered and dried to give 6.57 g of the desired compound as a solid (yield: 48%).
WORKUP
后处理
- temperatureheated
- temperatureto reflux for 1 hour
- temperatureto cool
- concentrationconcentrated
- additiondiluted with water
- customA precipitate was obtained
- filtrationthat was filtered
- customdried