The syntheses of 3-2 proceeded according to Scheme 19.
Tempone 3-1 (1.57 g, 9.22 mmol) and propargylamine (0.7 mL, 10.93 mmol) were dissolved in 1,2-dichloroethane (10 mL) to give a yellow solution. Acetic acid (0.67 mL, 10.95 mmols) was added causing an orange gelatinous precipitate. The reaction stirred under Argon for 24 h. Sodium triacetoxyborohydride (3.52 g, 16.6 mmol) was added neat and the reaction continued under Argon for 48 h after which the solvent was removed under reduced pressure leaving an orange oil. The oil was taken up in ethyl acetate (15 mL) and stirred at 40° C. for 1 h and then filtered. Florisil was added to the filtrate and the solvent removed under reduced pressure. Flash chromatography yielded 3-2 (1.542 g, 80%) as an orange solid.
Rf (ethyl acetate): 0.2
IR: 3400 cm−1, 3300 cm−1 and 3000 cm−1
m.p.: 65-67° C.
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