HRID1440449
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
A solution of ethyl (2-methyl-6-trifluoromethyl-3H-pyrimidin-4-on-5-yl)acetate (2.50 g, 9.46 mmol), N,N-dimethylaniline (3 drops), and phosphorus oxychloride (35 mL) was heated under reflux for 4.5 h. The mixture was concentrated, cooled, and ice water was added. Solid KOH was added to neutralize the mixture and it was extracted with ether. The combined extracts were washed with brine, dried (MgSO4), and concentrated to give 2.61 g (98%) of product as a yellow oil.
WORKUP
后处理
- temperatureunder reflux for 4.5 h
- concentrationThe mixture was concentrated
- temperaturecooled
- additionice water was added
- additionSolid KOH was added
- extractionwas extracted with ether
- washThe combined extracts were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated