HRID1594566

反应详情

EQUATION

反应方程式

HRID 1594566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3.8 g (26 mmol) of 2,5-dichloropyridine, 1.3 g (12 mmol) of sodium carbonate, 1.3 g (5.2 mmol) of (7RS,8aSR)-7-(4-fluorophenoxy)methyl-1,2,3,4,6,7,8,8a-octahydro-pyrrolo[1,2-a]pyrazine (Preparation 2), and 20 mL of isoamyl alcohol was heated at reflux for 18 hours. The solvent was evaporated, the residue taken up in water and ethyl acetate, and the pH adjusted to 11 with sodium carbonate. The layers were separated and the organic phase was dried (magnesium sulfate), filtered, and evaporated. Purification by medium pressure silica gel chromatography with ethyl acetate gave 35 mg (2%) of the title compound. Mp (.HCl) 202-206° C. HRMS calc'd for C19H21ClFN3O (MH+): 362.1435, found: 362.1451.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 18 hours
  3. customThe solvent was evaporated
  4. customThe layers were separated
  5. dry with materialthe organic phase was dried (magnesium sulfate)
  6. filtrationfiltered
  7. customevaporated
  8. customPurification by medium pressure silica gel chromatography with ethyl acetate