反应详情

温度

70 °C

To a dimethylformamide (4.5 ml, 60 mmol) at 0° C. was added phosphorous oxychloride (3 ml, 30 mmol). Tropinone (2 g, 13 mmol) was added, and the reaction mixture heated to 70° C. for 1/2 h After cooling, crushed ice was added and then solid potassium carbonate until alkaline reaction. The water solution was extracted with ether (3×30 ml). The ether extracts were dried and evaporated. The crude compound was purified by column chromatography with acetone as eluent. The title compound was precipitated with a 1M oxalic acid acetone solution, filtered and dried. M.p. 136°-137° C. decomposes.

1. temperatureAfter cooling
2. customcrushed ice
3. additionwas added
4. extractionThe water solution was extracted with ether (3×30 ml)
5. dry with materialThe ether extracts were dried
6. customevaporated
7. customThe crude compound was purified by column chromatography with acetone as eluent
8. customThe title compound was precipitated with a 1M oxalic acid acetone solution
9. filtrationfiltered
10. customdried