反应详情

1.54 g (4.25 mmol) of N-(4′-formylbiphenyl-3-ylmethyl)-N-methylbenzamide (prepared as in Example 1(e)), 20 ml of toluene, 0.56 g (4.25 mmol)) of dimethyl malonate and 123 mg (0.85 mmol) of piperidine acetate are introduced into a three-necked flask under a stream of nitrogen. The mixture is refluxed for 5 hours, while separating off the water formed using Dean-Stark apparatus. The reaction medium is cooled, extracted with ethyl acetate and washed with water. The organic phase is separated out after settling of the phases has taken place, dried over magnesium sulfate and evaporated. The crude product is purified by chromatography on a column of silica eluted with a mixture of heptane and ethyl acetate (70/30). After evaporation of the solvents, 1.4 g (75%) of the expected product are collected.

1. temperatureThe mixture is refluxed for 5 hours
2. customwhile separating off the water
3. customformed
4. temperatureThe reaction medium is cooled
5. extractionextracted with ethyl acetate
6. washwashed with water
7. customThe organic phase is separated out
8. dry with materialdried over magnesium sulfate
9. customevaporated
10. customThe crude product is purified by chromatography on a column of silica
11. washeluted with a mixture of heptane and ethyl acetate (70/30)
12. customAfter evaporation of the solvents, 1.4 g (75%) of the expected product
13. customare collected