HRID2084284

反应详情

EQUATION

反应方程式

HRID 2084284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 7-bromo-1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole (0.6 g, 1.8 mmol), prepared as described in example 4, and sodium thiophenate (0.3 g, 2.24 mmol) in dry N,N-dimethylformamide (10 ml) was stirred at room temperature for about 5 hours and then poured into brine and extracted with dichloromethane. The combined organic layers were washed with brine, dried over sodium sulfate end evaporated. The residue was chromatographed on silica gel (cyclohexane:ethyl acetate=90:10) to give 0.3 g (45% yield) of the title compound as a colourless solid which crystallized on standing.

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over sodium sulfate end
  4. customevaporated
  5. customThe residue was chromatographed on silica gel (cyclohexane:ethyl acetate=90:10)