反应详情

温度

140 °C

Under nitrogen, titanium tetrachloride (0.9 ml, 8.2 mmol) was added to the above enamine (Example 33) (1.5 g, 7.5 mmol) and the stirred mixture was heated at 140° C. for 1 hour. After cooling, 10M-sodium hydroxide solution (20 ml) was added and the mixture heated under reflux for 1 hour. After being allowed to cool, this mixture was filtered and the solids washed with dichloromethane. Any organics in the filtrate were also extracted into dichloromethane. All extracts were combined, dried (Na2SO4), filtered and the solvent evaporated. Kugelrohr distillation (175° C., 0.05 mmHg) gave the product as a pale yellow powder.

1. temperatureAfter cooling
2. temperaturethe mixture heated
3. temperatureunder reflux for 1 hour
4. temperatureto cool
5. filtrationthis mixture was filtered
6. washthe solids washed with dichloromethane
7. extractionAny organics in the filtrate were also extracted into dichloromethane
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. customthe solvent evaporated
11. distillationKugelrohr distillation (175° C., 0.05 mmHg)