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0042160835
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note
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Discover focused microwave oven from CEM was used for our study.
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Petke, J.D.11
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34
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0042661865
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note
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(b) Jacobsen et al. reported the solution phase synthesis of 1,2,3,4-tetrahydroquinoxalin-2-ones using similar cyclization. They observed primary amino group stands to be more nucleophilic than adjacent substituted NH group. Probably steric hindrance of t-butyl group is the key factor to facilitate the acid chloride to opt primary amine in their work (Scheme 3).
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35
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0042160831
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note
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2O and dried in vacuum. Polymer support of 8m was cleaved by exposing it to microwave (150 W) for 10 min in sodium methoxide solution. Progress of cleavage was monitored on TLC [solvent: EtOAc-n-hexane (1:2)]. Separation of 2-arm PEG from the desired products was achieved by precipitation in ethanol to give crude mixtures of compounds 9m and 10m in 90% combined yield and 93% (53% and 40%) HPLC purity (UV detection at λ = 254 nm. Column: Sphereclone 5u Si (250 x 4.6 nm); gradient: 50% EtOAc/n-hexane; flow rate: 1 mL/min).
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