HRID1440449

反应详情

EQUATION

反应方程式

HRID 1440449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder reflux for 4.5 h
  2. concentrationThe mixture was concentrated
  3. temperaturecooled
  4. additionice water was added
  5. additionSolid KOH was added
  6. extractionwas extracted with ether
  7. washThe combined extracts were washed with brine
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated