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33644992802
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note
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2O (0.25 g, 1 mmol), Baylis-Hillman acetate 1 (1 mmol), and anhyd MeOH (15 mL). The mixture was stirred at r.t. for 4-8 h. Then, to the resultant mixture was added silica gel powder (2.0 g). After evaporation of the solvent, the silica gel-absorbed crude product was loaded to chromatography column for further purification using MeOH-EtOAc (1:1) as eluent.
-
-
-
-
52
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0001420970
-
-
1H NMR spectrum of a trisubstituted alkene the β-vinylic proton, cis and trans to the ester group are known to resonate at δ = 7.5 ppm and δ = 6.5 ppm, respectively, when alkene is substituted by an aryl group; while the same proton cis and trans to an ester group appears at δ = 6.8 ppm and δ = 5.7 ppm, respectively, when substituted by an alkyl one. See: (a) Larson, G. L.; de Kaifer, C. F.; Seda, R.; Torres, L. E.; Ramirez, J. R. J. Org. Chem. 1984, 49, 3385.
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55
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56
-
-
33645008290
-
-
note
-
2: C, 42.57; H, 3.57. Found: C, 42.89; H, 3.65.
-
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-
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57
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24044470646
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Li, C. J. Chem. Rev. 2005, 105, 3095.
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33644992801
-
-
note
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4. After evaporation of solvent, the residue was purified by chromatography using cyclohexane-EtOAc (6:1) as eluent.
-
-
-
-
59
-
-
33644996185
-
-
note
-
3S: C, 64.72; H, 6.52. Found: C, 64.96; H, 6.62.
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-
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