Erreaktibo organolitikoak sintesi asimetrikoan, aminen ...
Erreaktibo organolitikoak sintesi asimetrikoan, aminen ...
Erreaktibo organolitikoak sintesi asimetrikoan, aminen ...
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S. Arrasate Doktorego-Tesia<br />
nahastea inguruneko tenperaturara heltzen utzi zen. Ondoren, NaCl-ko disoluzio aseaz<br />
(3 × 10 mL) garbitu zen eta fase organikoa Na2SO4 anhidroz lehortu, iragazi eta<br />
kontzentratu zen, solido marroi bat bezala 2a lortu zelarik. Produktu hau Flash<br />
kromatografia dela medio purifikatu zen (silize-gela, hexano/AcOEt %20) 2a (115 mg,<br />
0.5 mmol) lortu zelarik.<br />
Ph<br />
HN<br />
Me<br />
OCH<br />
3<br />
Etekina: %99.<br />
[α]D 20 : +9.7 (c = 1.1, EtOH).<br />
Bib. 6 [α]D 20 : +27.1 (c = 1.2, EtOH).<br />
es: %34.<br />
U.p.: 64-65 o C (hexano).<br />
Bib. 7 61-62 o C<br />
es: %34 (Chiralcel OD, hexano/2-propanol %2, 0.5 mL/min, tr (R) = 21.8 min (%67.1);<br />
tr (S) = 24.3 (%32.9).<br />
1 H-NMR (δ, ppm): 1.65 (d, J = 6.7 Hz, 3H, CH3), 3.83 (s, 3H, OCH3), 3.98 (s, 1H,<br />
NH), 4.59 (q, J = 6.7 Hz, 1H, -CH-NH), 6.66 (d, J = 8.9 Hz, 2H, H2, H6), 6.89 (d, J =<br />
8.9 Hz, 2H, H3, H5), 7.41-7.54 (m, 5H, Harom).<br />
13 C-NMR (δ, ppm): 24.8 (CH3), 53.9 (CH-NH), 55.3 (OCH3), 114.3 (C2, C6), 114.5<br />
(C3,C5), 125.7 (C2’, C6’), 126.6 (C4’), 128.4 (C3’, C5’), 141.4 (C1), 145.3 (C1’), 151.6<br />
(C4).<br />
IR (CHCl3): 3389 (N-H), 1513 (C=C), 1237 (C-N) cm -1 .<br />
E.M. (IE) [m/z (ugaritasun erlatiboa)]: 227 (M + , 71), 212 (81), 168 (5), 123 (64), 108<br />
(66), 105 (100), 77 (32).<br />
Analisi elementala: C15H17NO<br />
158<br />
Kalkulatua: %C: 79.26 %H: 7.54 %N: 6.16<br />
Lortutakoa: %C: 79.22 %H: 7.60 %N: 6.15<br />
7 Denmark. S. E.; Nakajima, N.; Nicaise, O. J.-C. J. Am. Chem. Soc. 1994, 116, 8797.