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•- to form the [4 + 2]cycloadduct, see: (a) Kotani, H.; Ohkubo, K.; Fukuzumi, S. J. Am. Chem. Soc. 2004, 126, 15999.
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•- to form the [4 + 2]cycloadduct, see: (a) Kotani, H.; Ohkubo, K.; Fukuzumi, S. J. Am. Chem. Soc. 2004, 126, 15999.
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37
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33846178315
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Typically, a chloroform solution (10 mL) containing Acr+-Mes (12 mg, 2.9 × 10-5 mol) and DMA (60 mg, 2.9 × 10 -4 mol) in a Schlenk flask with a rubber septum was degassed by freeze-pump-thaw cycle three times and flushed with argon gas. The solution was then irradiated with a 500 W xenon lamp (Ushio Optical ModelX SX-UID 500XAMQ) through a color filter glass (Asahi Techno Glass Y43) transmitting λ > 430 nm at 298 K. After 4 h photoirradiation, dimethyllepidopterene was isolated by silica gel column chromatography (hexane/toluene 1/1, v/v) as pale yellow solid (12% yield, Dimethyllepidopterene: Anal. Calcd for C32H 26·0.8(H2O) C, 90.44; H, 6.55; found C, 90.59; H, 6.32. 1H NMR (300 MHz, CDCl3) δ 7.33 (d, J, 7.5 Hz, 4H, 7.02 (t, J, 7.5 Hz, 4H, 6.80 (t, J, 7.5 Hz, 4H, 6.72 (d, J, 7.5 Hz, 4H, 2.71 (s, 4H, 2.22 s, 6H, 13
-
2 calcd 288.1, found 288.4.
-
-
-
-
38
-
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0242389581
-
-
-1, R1 = 0.040 (I > 2σ(I)), Rw = 0.105 (all data), GOF = 1.121. For details, see Supporting Information (CIF file). A similar crystal structure has been reported briefly: Liu, Q.-X.; Song, H.-B.; Xu, F.-B.; Li, Q.-S.; Zeng, X.-S.; Leng, X.-B.; Zhang, Z.-Z. J. Chem. Res., Synop. 2003, 445.
-
-1, R1 = 0.040 (I > 2σ(I)), Rw = 0.105 (all data), GOF = 1.121. For details, see Supporting Information (CIF file). A similar crystal structure has been reported briefly: Liu, Q.-X.; Song, H.-B.; Xu, F.-B.; Li, Q.-S.; Zeng, X.-S.; Leng, X.-B.; Zhang, Z.-Z. J. Chem. Res., Synop. 2003, 445.
-
-
-
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39
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33846139089
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-
+-Mes.
-
+-Mes.
-
-
-
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40
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33846174395
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-
-1 of sweep rate.
-
-1 of sweep rate.
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-
-
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41
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0033576856
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33846160253
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18a
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18a
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44
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46
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33846152392
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16
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16
-
-
-
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47
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33846165556
-
-
18b
-
18b
-
-
-
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48
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20744439680
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