HRID361836

反应详情

EQUATION

反应方程式

HRID 361836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,5-Difluoronitrobenzene (2.69 ml, 24.84 mmol), 1-benzyl-4-methylaminopiperidine (EXAMPLE 9, 5.00 g, 24.84 mmol), and potassium carbonate (4.12 g, 29.81 mmol) are refluxed in acetonitrile for 21 hr. The mixture is then poured into water and extracted with chloroform. The extract is dried over sodium sulfate, filtered and concentrated. The concentrate is chromatographed (silica gel; ethyl acetate/hexane) to give the title compound, NMR (300 MHz, CD3OD) 7.45, 7.37, 7.29, 3.46, 2.99, 2.87, 2.64, 1.98 and 1.67δ.

WORKUP

后处理

  1. extractionextracted with chloroform
  2. dry with materialThe extract is dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe concentrate is chromatographed (silica gel; ethyl acetate/hexane)