反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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 h. 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 calcd for C19H21 ClFN3O (MH+): 362.1435, found: 362.1451.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for 18 h
- customThe solvent was evaporated
- customThe layers were separated
- dry with materialthe organic phase was dried (magnesium sulfate)
- filtrationfiltered
- customevaporated
- customPurification by medium pressure silica gel chromatography with ethyl acetate