反应详情

A mixture of (±)-4-(4-chlorobenzyl)-2-chloromethyimorphoiine (10.0 g 38.5 mmol), 4-chloro-2-methoxyphenol (9.0 g, 58 mmol), potassium ethoxide (6.5 g, 77 mmol), and 18-crown-6 (10.2 g, 38.5) was refluxed in toluene (100 ml) for 34 h. Water (200 ml) was added and the phases were separated. Drying and evaporation of the toluene phase was followed by column chromatography on silica gel with 3% ethanol in dichloromethane as eluent. The free base was dissolved in ether and precipitated with oxalic acid to give the title compound. Yield 10.3 g, 57%, mp 133-139° C.

1. customthe phases were separated
2. customDrying
3. customevaporation of the toluene phase
4. dissolutionThe free base was dissolved in ether
5. customprecipitated with oxalic acid