Table 1. Optimization of the Reaction Times.
Entry | Reaction time | 4 Yield (%) | Entry | Reaction time | 4 yield (%) | |
---|---|---|---|---|---|---|
1 | 0 min | 2.00 | 11 | 2 h | 2.95 | |
2 | 10 min | 2.46 | 12 | 3 h | 3.00 | |
3 | 20 min | 2.77 | 13 | 4 h | 3.01 | |
4 | 30 min | 2.87 | 14 | 5 h | 2.74 | |
5 | 40 min | 3.35 | 15 | 6 h | 2.67 | |
6 | 50 min | 3.42 | 16 | 7 h | 2.63 | |
7 | 60 min | 3.86 | 17 | 8 h | 2.54 | |
8 | 70 min | 3.64 | 18 | 9 h | 2.46 | |
9 | 80 min | 3.53 | 19 | 10 h | 2.38 | |
10 | 90 min | 3.20 | 20 | 11 h | 2.10 |
*Reaction conditions: (−)-Sclareol 1 (10 mmol), Na2WO4·2H2O (0.1 equiv), NaH2PO4 (0.1 equiv), TBAB (0.1 equiv), 1, 4-dioxane (7 mL), H2O2 (5 mL), 70 °C, 2 h; then rising to 90 °C; TBAB (Tetrabutyl ammonium bromide); GC yield.
Reaction time starts counting when the reaction system temperature rises to 90 °C.