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58149338426
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Microwave experiments were conducted in open reaction vessels of a Synthwave 402 reactor manufactured by M/s Prolabo, 54 rue Roger Salengro, Cedex, France. The temperature of the reaction mixture was set at 140°C and measured by a computer controlled sensor using 80% power (maximum output 300 Watts) with an operating frequency of 2.45 GHz. The reaction time specified is the total irradiation time. The hold time at final temperature is 25% of the total time.
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Microwave experiments were conducted in open reaction vessels of a Synthwave 402 reactor manufactured by M/s Prolabo, 54 rue Roger Salengro, Cedex, France. The temperature of the reaction mixture was set at 140°C and measured by a computer controlled sensor using 80% power (maximum output 300 Watts) with an operating frequency of 2.45 GHz. The reaction time specified is the total irradiation time. The hold time at final temperature is 25% of the total time.
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46
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58149334012
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Spectral and Analytical Data of Selected Compounds: Compound B: mp 97-99°C; Rf, 0.7 (EtOAc-hexane, 10:90, IR (KBr, 3059, 3028, 2922, 1686, 1653, 1606, 1448, 1217, 1180, 1010, 755 cm-1. 1H NMR (300 MHz, CDCl3, δ, 8.01 (d, 2 H, J, 7.4 Hz, 7.92 (d, 2 H, J, 7.4 Hz, 7.88 (d, 2 H, J, 8.0 Hz, 7.18-7.54 (m, 6 H, 5.25 (s, 1 H, 4.84 (s, 2 H, 2.40 (s, 3 H, 13C NMR (75 MHz, CDCl3, δ, 196.0, 190.5, 152.7, 152.0, 143.3, 141.7, 136.9, 136.2, 134.2, 132.9, 132.4, 129.1, 129.0, 128.5 (2 x C, 128.4, 128.3, 128.2, 128.2, 128.0, 126.5, 123.3, 42.7, 21.4. MS (ESI, m/z, 341 [M, 1, Compound 3a: mp 135-36°C; Rf, 0.8 (EtOAc-hexane, 10:90, IR (KBr, 3035, 2924, 1595, 1550, 1495, 1449, 1180, 756 cm-1. 1H NMR (300 MHz, CDCl3, δ, 8.21 (m, 4 H, 7.89 (s, 2 H, 7.75 d, 2 H, J, 7.0
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+ + 1].
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