反应详情

600 mg (1.8 mmol) of N-(4′-formylbiphenyl-3-ylmethyl)-N-methylbenzamide (prepared as in Example 1(e)), 10 ml of toluene, 300 μl (1.8 mmol) of diethyl malonate and 50 mg (0.35 mmol) of piperidine acetate are introduced into a three-necked flask under a stream of nitrogen. This mixture is refluxed for 6 hours, while separating out 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 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 (75/25). After evaporation of the solvents, 700 mg (84%) of expected product are collected.

1. temperatureThis mixture is refluxed for 6 hours
2. customwhile separating out 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 after settling
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 (75/25)
12. customAfter evaporation of the solvents, 700 mg (84%) of expected product
13. customare collected