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52949093431
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Selected Physical and Spectroscopic Data Compound 10: [α]D25 +86 (c 0.9, MeOH, 1H NMR (300 MHz, MeOD, δ, 7.61 (d, J, 2.0 Hz, 1 H, 7.12 (dd, J, 8.3, 2.0 Hz, 1 H, 6.84 (d, J, 8.3 Hz, 1 H, 5.47 (s, 1 H, 2.66 (s, 3 H, 1.48 (s, 9 H) ppm. HRMS (ES, m/z calcd for C 14H18NO5NaI [M, Na, 430.0127; found: 430.0128. Compound 5: [α]D25 +16(c 1.0, CHCl3, 1H NMR (300 MHz, CDCl 3, 1:1 mixture of retainers, δ, 7.72 and 7.71 (d, J, 2.2 Hz, 1 H, 7.42 and 7.30 (d, J, 2.3 Hz, 1 H, 7.29-7.24 (m, 0.5 H, overlapped with solvent, 7.22 (dd, J, 8.5, 2.2 Hz, 0.5 H, 7.22 (dd, J, 8.5, 2.2 Hz, 0.5 H, 7.10 (dd, J, 8.5, 2.2 Hz, 0.5 H, 6.78 (d, J, 8.5 Hz, 1 H, 6.71 (d, J, 8.5 Hz, 1 H, 6.58-6.32 m, 1 H, 6.54 an
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- 823.4242; found: 823.4269.
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26
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52949114107
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Abbreviations: DEPBT, 3-(diethyloxyphosphoryloxy)-1,2,3-benzotriazin-4 (3H)-one; EDC, 1-[3-(eimethyl-amino)propyl]-3-ethylcarbodiimide; HOBt, N-hydroxybenzotriazole, SPhos, 2-dicyclohexylphosphino-2′, 6′-dimethoxybiphenyl; MOP, diphenylphosphino)-2′-methoxy-1, 1′-binaphtyl; NMP, N-methylpyrolidinone
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Abbreviations: DEPBT = 3-(diethyloxyphosphoryloxy)-1,2,3-benzotriazin-4 (3H)-one; EDC = 1-[3-(eimethyl-amino)propyl]-3-ethylcarbodiimide; HOBt = N-hydroxybenzotriazole, SPhos = 2-dicyclohexylphosphino-2′, 6′-dimethoxybiphenyl; MOP = (diphenylphosphino)-2′-methoxy-1, 1′-binaphtyl; NMP = N-methylpyrolidinone.
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Microwave experiments were conducted using a Discover microwave reactor from CEM. All experiments were performed in sealed tubes (capacity 10 mL) under argon atmosphere. Microwave irradiation of 300 W was used, the temperature being ramped from r.t. to 90°C or 110°C in 1 min. Once this temperature was reached, the reaction mixture was held at 90°C or 110°C for the indicated time.
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Microwave experiments were conducted using a Discover microwave reactor from CEM. All experiments were performed in sealed tubes (capacity 10 mL) under argon atmosphere. Microwave irradiation of 300 W was used, the temperature being ramped from r.t. to 90°C or 110°C in 1 min. Once this temperature was reached, the reaction mixture was held at 90°C or 110°C for the indicated time.
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