Table 2.
Screening and control experiment of gram-scale [2 + 2] dimerization of α-asarone catalyzed by UCN under white lighta.
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|---|---|---|---|---|
| Entry | Light | Reactor | Reaction condition variations | Yieldb |
| 1 | + | Batch | UCN powdersc | 48% |
| 2 | + | Flow | UCN@glass fibersd | 70% |
| 3 | + | Flow | UCN@glass beads | 81% |
| 4 | − | Flow | In dark | Trace |
| 5 | + | Flow | In acetonitrile | 2%e |
| 6 | + | Batch | UCN@glass beads | 53% |
| 7f | + | Flow | UCN@glass beads | 87% |
aStandard reaction conditions of flow system: (α-asarone) = 0.167 m, VCH3NO2 = 60 mL, white LED lamp (0.1 W/cm2), room temperature, air, irradiation time 48 h.
bIsolated yield.
cThe amount of UCN is 200 mg.
dThe amount of UCN coated on glass fibers is 80 mg.
eConversion from GC-MS.
fUsing a photoreactor assembled from six paralleled glass tubes with irradiation time 8 h.
