rated, combined with the filtrate from the second crystallization, and recrystallized from EtOAc
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and recrystallized from EtOAc giving 0.22 g nf yellow crystals, m p 237-239". 'This was found by ir, nrnr. and uv spectra to have the structure 15. The principal spectral bands are: ir 172.5. 16M I C .Oj and 1620, 1590. 1580 c m (C(E tOH) 220 nip i f 32.050), 265 (19,250). y374 (5150); h 3.22 and 3.24 (2 s. 6. NCH3). 6.42 I S . 1 . ,?-=CHI. and between 6.75 and 7.65 (m's. 7. arom H's). Column fractions 10--17 were evaporated giving 0.2 g of nearly white solid. This was recrystallized from i-PrOH yielding 0.18 g of white needles. mp 226--228.5". Ir. nmr. and analysis showed this to have the structure 16. The principal spectral hands are: ir (Nujol mull) 1740. (C-0) and 1610. 1590. 1570 cm ( C = ~ N , / C z C i : nnir iCI)C13) 6 1.8 (d . X. 5-CH3j. 3.39 is, 3, N('H3'!. 4.14 l q . I . <i-CH). and between '7.05 and 7.65 (m's . 7. arom H's)
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rated, combined with the filtrate from the second crystallization, and recrystallized from EtOAc
and recrystallized from EtOAc giving 0.22 g nf yellow crystals, m p 237-239". 'This was found by ir, nrnr. and uv spectra to have the structure 15. The principal spectral bands are: ir 172.5. 16M I C .Oj and 1620, 1590. 1580 c m (C(E tOH) 220 nip i f 32.050), 265 (19,250). y374 (5150); h 3.22 and 3.24 (2 s. 6. NCH3). 6.42 I S . 1 . ,?-=CHI. and between 6.75 and 7.65 (m's. 7. arom H's). Column f...
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