HRID512451

反应详情

EQUATION

反应方程式

HRID 512451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe mixture was then heated
  2. temperatureunder reflux for 2 h
  3. concentrationThe mixture was concentrated to about 15 ml
  4. washwashed with dichloromethane
  5. additionthe aqueous phase was adjusted to pH 2 by addition of 2N hydrochloric acid
  6. extractionThe mixture was again extracted with dichloromethane
  7. customthe organic phase was dried
  8. concentrationconcentrated