反应详情

温度

120 °C

To compound 1a (3.363 g) was added 10% HCl solution (40 mL) and refluxed at 120° C. for 30 min. The reaction mixture was then kept at RT for 24 hours. The white lumps formed were filtered. The filtrate was extracted with hexane (50 mL, 2×) and the extracts added to the white lumps after removal of solvent. It was dried in a vacuum dessicator for 24 hours to obtain 2a which was quantitative. 1H NMR (in CDCl3): δ in ppm 0.83-0.87 (3H, m), 1.23 (26H, m), 1.52-1.55 (2H, m), 2.67 (1H, D2O exchangeable), 3.42-3.51 (4H, m), 3.60-3.70 (2H, m), 3.84-3.85 (1H, m), 6.63-6.70 (1H, D2O exchangeable); 13C NMR (in CDCl3): δ in ppm 14.6, 23.1, 26.5, 29.8, 29.9, 30.0, 30.1, 30.2, 32.4, 64.5, 71.0, 72.3, 72.9.

1. customThe white lumps formed
2. filtrationwere filtered
3. extractionThe filtrate was extracted with hexane (50 mL, 2×)
4. additionthe extracts added to the white lumps
5. customafter removal of solvent
6. customIt was dried in a vacuum dessicator for 24 hours