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14
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15844382173
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note
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THF or methylene chloride are typically used solvents.
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15
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15844396636
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note
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Isolation of a dry solid was only possible by addition of an ethyl acetate solution of 13 to a large excess of tert-butyl methyl ether at low temperature (-15 to 20°C).
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16
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15844365713
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note
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Initially, the HCl salt precipitation was unsuccessful in either dioxane or toluene due to the residual DCHA, because the free base of D-Abu had not been used. Once this was recognized and rectified, the HCl salt was easily produced as long as both water and ethyl acetate were removed via initial azeotropic distillation with dioxane.
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18
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