HRID512451
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
At room temperature, 4.73 g (21.4 mmol) of methyl 2-oxo-6-(trifluoromethyl)-1,2-dihydropyridine-3-carboxylate were dissolved in 45 ml of methanol and 15 ml of water, 1.80 g (42.8 mmol) of lithium hydroxide monohydrate were added and the mixture was then heated under reflux for 2 h. The mixture was concentrated to about 15 ml and then washed with dichloromethane and the aqueous phase was adjusted to pH 2 by addition of 2N hydrochloric acid. The mixture was again extracted with dichloromethane, and the organic phase was dried and concentrated. This gave 4.2 g (94% of theory) of a colorless powder.
WORKUP
后处理
- temperaturethe mixture was then heated
- temperatureunder reflux for 2 h
- concentrationThe mixture was concentrated to about 15 ml
- washwashed with dichloromethane
- additionthe aqueous phase was adjusted to pH 2 by addition of 2N hydrochloric acid
- extractionThe mixture was again extracted with dichloromethane
- customthe organic phase was dried
- concentrationconcentrated