HRID635893

反应详情

EQUATION

反应方程式

HRID 635893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(Step 2) In 85 ml of dry tetrahydrofuran was dissolved 17 g of 2,4-dichloro-6-phenyl-1,3,5-triazine. To this solution on an ice-water bath was added 135 ml of 1M methylmagnesium bromide-tetrahydrofuran dropwise over about 30 minutes. After completion of dropwise addition, the mixture was stirred at room temperature for 2 hours. This reaction mixture was poured into iced water and extracted with ethyl acetate. The extract was washed with water, dried over MgSO4, and concentrated. The residue was purified with silica gel column chromatography to provide 3.6 g of the title compound as white crystals.

WORKUP

后处理

  1. additionAfter completion of dropwise addition
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue was purified with silica gel column chromatography