反应详情

温度

90 °C

To a suspension of 2 (11.3 g, 44.9 mmol) in dioxane was added perchloric acid (11.4 ml, 0.14 mol) and the reaction was heated at 90° C. under N2 for 1 hour. The reaction was cooled, neutralised with 2M NaOH (75 ml) and filtered. The aqueous layer was extracted with DCM (4×30 ml) and the organic layers were combined and dried over MgSO4. The organic layer was further treated with charcoal and filtered through celite. The dark yellow filtrate was evaporated in vacuo, and the resulting solid was triturated with hexane (50 ml) and dried to give 3 (7.3 g, 75%) as a light yellow powder. m/z (LC-MS, ESP): 216 (M++1). 1H-NMR (300 MHz, DMSO-d6): 3.3 (t, 4H), 3.65 (t, 4H), 5.4 (d, 1H), 6.25 (d, 1H).

1. temperatureThe reaction was cooled
2. filtrationfiltered
3. extractionThe aqueous layer was extracted with DCM (4×30 ml)
4. dry with materialdried over MgSO4
5. additionThe organic layer was further treated with charcoal
6. filtrationfiltered through celite
7. customThe dark yellow filtrate was evaporated in vacuo
8. customthe resulting solid was triturated with hexane (50 ml)
9. customdried