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26
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52049093541
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note
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1f was heated at 250 °C under nitrogen. The internal pressure reached ca. 7 MPa. The mixture was heated at the same temperature for 4 h. After cooling, the solution was washed with water, dried, and evaporated. The residue was chromatographed (hexane) on silica gel to give 2, 3, and 4 in 52, 9, and 3% yields, respectively. Compound 1 was recovered in 15% yield (Table 1, entry 1). Caution: Attention should be paid for the leak of the gas, since a large amount of harmful chlorine was evolved during the reactions. It is important to firmly tighten the screw of the stainless autoclave. The operation should be carried out in a well-ventilated fume hood when the autoclave is opened. Many times use of the stainless autoclave should be avoided because of the rust caused by chlorine gas.
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29
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33947337573
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33
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0039738319
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34
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52049087676
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Gregoire, J. H. C. M. A. U.S. Patent 3,894,923, 1975.
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38
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52049100469
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note
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4: C, 44.92; H, 6.85. Found: C, 44.83; H, 7.00.
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39
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52049121141
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note
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4: C, 44.92; H, 6.85. Found: C, 44.64; H, 6.74.
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-
-
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40
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52049115510
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note
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4: C, 44.16; H, 3.71. Found: C, 44.40; H, 3.73.
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41
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33745031820
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Tisserand S., Bejot R., Billaud C., Li D.R., Falck J.R., and Mioskowski C. Tetrahedron Lett. 47 (2006) 5177-5180
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Mioskowski, C.6
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