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REPRINTS
3744
JAIME-FIGUEROA ET AL.
column chromatography (silica gel, hexane–EtOAc, 9:1). 1.8 g (84%) of
pure 3d was obtained as a solid; mp 109–110ꢀC (CH2Cl2–hexane);
1H NMR (DMSO-d6) d 1.53 (s, 9H, -t-Bu), 1.87 (s, 3H, -Me), 4.97 (s, 2H,
-Bn), 7.15–7.45 (m, 5H, -Ph), 7.87 (s, 1H, H-6); Anal. calc. for C17H20N2O4:
C, 64.53; H, 6.37; N, 8.85. Found: C, 64.27; H, 6.30; N, 8.72.
3a: Mp 108ꢀC (CH2Cl2–hexane); H NMR (DMSO-d6) d 1.52 (s, 9H,
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-t-Bu), 4.96 (s, 2H, -Bn), 5.9 (d, 1H, H-5, J ¼ 8.3) 7.17–7.40 (m, 5H, -Ph),
7.98 (s, 1H, H-6, J ¼ 8.3); Anal. calc. for C16H18N2O4: C, 63.56; H, 6.00; N,
9.26. Found: C, 63.69; H, 6.04; N, 9.19.
3b: Mp 70–71ꢀC (CH2Cl2–hexane); H NMR (DMSO-d6) d 0.83 (d,
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6H, i-Bu), 1.53 (s, 9H, -t-Bu), 1.99 (m, 1H, -CH(Me)2), 3.61 (d, 2H,
i-Pr-CH2-), 5.82 (d, 1H, H-5, J ¼ 8.3), 7.92 (d, 1H, H-6, J ¼ 8.3); Anal.
calc. for C33H20N2O4: C, 58.19; H, 7.51; N, 10.44. Found: C, 58.20; H, 7.74;
N, 10.23.
3c: Oil; 1H NMR (DMSO-d6) d 1.53 (s, 9H, -t-Bu), 4.36 (m, 2H, -allyl),
5.1 (m, 2H, vinyl), 5.71–5.90 (m, 1H, vinyl), 5.84 (d, 1H, H-5, J ¼ 8.3) 7.95
(d, 1H, H-6, J ¼ 8.3); Anal. calc. for C12H16N2O4: C, 57.12; H, 6.39; N,
11.10. Found: C, 57.40; H, 6.45; N, 11.12.
3e: Mp 81–82ꢀC (CH2Cl2–hexane); 1H NMR (DMSO-d6) d 0.82 (d, 6H,
-i-Bu), 1.53 (s, 9H, -t-Bu), 1.85 (s, 3H, -Me), 1.90–2.08 (m, 1H, -CH(Me)2),
3.63 (d, 2H, i-Pr-CH2-), 7.81 (s, 1H, H-6); Anal. calc. for C14H22N2O4: C,
59.55; H, 7.85; N, 9.92. Found: C, 59.70; H, 8.01; N, 9.67.
3f: Mp 55ꢀC (hexane); 1H NMR (DMSO-d6) d 1.53 (s, 9H, -t-Bu), 1.85
(s, 3H, -Me), 4.38 (m, 2H, -allyl), 5.03–5.13 (m, 2H, vinyl), 5.79–5.90 (m,
1H, vinyl), 8.84 (s, 1H, H-6); Anal. calc. for C33H18N2O4: C, 58.63; H, 6.81;
N, 10.52. Found: C, 58.79; H, 6.86; N, 10.15.
3g: Mp 115–116ꢀC (hexane); 1H NMR (DMSO-d6) d 1.53 (s, 9H, -t-Bu),
5.00 (s, 2H, -Bn), 7.15–7.40 (m, 5H, -Ph), 8.36 (s, 1H, H-6); Anal. calc.
for C16H17N2BrO4: C, 50.40; H, 4.49; N, 7.34. Found: C, 50.22; H, 4.43;
N, 7.17.
3h: Mp 86–88ꢀC (hexane); 1H NMR (DMSO-d6) d 1.54 (s, 9H, -t-Bu),
4.41 (d, 2H, -allyl), 5.15 (m, 2H, vinyl), 5.70–5.90 (m, 1H, vinyl), 8.33 (s, 1H,
H-6); Anal. calc. for C12H15N2BrO4.0.04 hex.; C, 43.98; H, 4.59; N, 8.38.
Found: C, 44.00; H, 4.59; N, 8.38.
3i: Oil; 1H NMR (DMSO-d6) d 1.54 (s, 9H, -t-Bu), 3.68 (s, 3H, -OMe)
4.38 (d, 2H, -allyl), 5.09 (m, 2H, vinyl), 5.70–5.89 (m, 1H, vinyl), 7.43 (s, 1H,
H-6); Anal. calc. for C33H18N2O5: C, 55.30; H, 6.42; N, 9.92. Found: C,
55.22; H, 6.63; N, 9.78.
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3j: Oil; H NMR (DMSO-d6) d 0.87 (t, 3H, -Me), 1.40–1.60 (m, 2H,
Me-CH2-C), 1.53 (s, 9H, -t-Bu), 2.26 (t, 2H, -CH2-Et), 4.38 (d, 2H, -allyl),
5.12 (m, 2H, vinyl), 5.70–5.93 (m, 1H, vinyl), 7.76 (s, 1H, H-6); Anal. calc. for
C15H22N2O4: C, 61.20; H, 7.53; N, 9.52. Found: C, 61.42; H, 7.83; N, 9.45.