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HETEROCYCLES, Vol. 68, No. 4, 2006
(3R,8aR)-3-Phenyltetrahydrothiazolo[3,4-a]pyrazine-5,8-dione (4a) was obtained as a white solid
(47%). mp 225-227 °C (from dichloromethane-ethyl ether).. IR (KBr) 1295, 1639, 1678 and 3257 cm-1;
1H NMR δ: 3.34-3.36 (2H, m), 3.55 (3H, s), 3.62-3.81 (1H, m), 4.13-4.21 (1H, m), 4.78 (1H, approx. t, J
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= 6.6 Hz), 6.43 (1H, s), 7.27-7.38 (5H, Ar-H); C NMR δ: 34.7, 46.2, 60.3, 64.7, 126.8, 128.6, 128.7,
139.1, 161.1, 166.3; MS (EI) m/z 248 (M+, 100%), 177 (25), 121 (36) and 77 (16). Anal. Calcd for
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C12H12N2O2S: C, 58.05; H, 4.87; N, 11.28. Found: C, 57.77; H, 5.23; N, 11.30%.
CH2Cl2).
= + 310 (c = 0.5,
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D
(3R,8aR)-3-Phenyl-7-prop-2-ynyltetrahydrothiazolo[3,4-a]pyrazine-5,8-dione (4b) was obtained as a
white solid (72%). mp 122.2-123.8 °C (from ethyl acetate-hexane). IR (KBr) 1676, 2123, 3228 and 3288
cm-1; 1H NMR δ: 2.34 (1H, t, J = 2.5 Hz) 3.38 (1H, dd, J = 6.0 and J = 12.9 Hz) 3.46-3.53 (1H, m), 4.08
(1H, d, J = 17 Hz), 4.21 (1H, dd, J = 2.5 and J = 17.5 Hz), 4.26 (1H, d, J = 17 Hz), 4.47 (1H, dd, J = 2.5
and J = 17.5 Hz), 4.63 (1H, ddd, J = 0.9, J = 6.0 and J = 12.9 Hz) 6.25 (1H, s), 7.17-7.20 (2H, m, Ar-H),
7.26-7.35 (3H, m, Ar-H); 13C NMR δ: 31.1, 34.9, 51.0, 63.6, 64.8, 73.3, 76.5, 125.1, 128.2, 128.8, 141.2,
163.5, 165.9; MS (EI) m/z 286 (M+, 100%), 162 (23), 121 (34) and 77 (10). Anal.: Calcd. for
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C15H14N2O2S: C, 62.92; H, 4.93; N, 9.78. Found: C, 62.58; H, 5.07; N, 9.87%.
2Cl2).
= + 115 (c = 1, CH-
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(3R,8aR)-7-Methoxycarbonylmethyl-3-phenyltetrahydrothiazolo[3,4-a]pyrazine-5,8-dione (4c) was
obtained as a white solid (37%). mp 118.5-120.7 °C (from ethyl acetate-hexane). IR (KBr) 1677, 1745
1
and 2961 cm-1; H NMR δ: 3.37 (1H, dd, J = 5.8 and J = 12.3 Hz), 3.51 (1H, dd, J = 10.1 and J = 12.3
Hz), 3.79 (3H, s), 3.83 (1H, d, J = 17.6 Hz), 4.02 (1H, d, J = 17.6 Hz), 4.70 (1H, dd, J = 5.8 and J = 10.1
Hz), 6.23 (1H, s), 7.21-7.23 (2H, m, Ar-H), 7.25-7.28 (1H, m, Ar-H), 7.32-7.34 (2H, m, Ar-H); 13C NMR
δ: 30.8, 47.3, 52.7, 53.2, 63.4, 64.7, 125.0, 128.2, 128.8, 141.1, 163.4, 167.1, 168.33; MS (EI) m/z 320
(M+, 100%), 302 (18), 177 (28), 121 (35), 102 (42) and 77 (89). Anal.: Calcd. for C15H16N2O4S: C, 56.24;
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H, 5.03; N, 8.74. Found: C, 56.11; H, 5.10; N, 8.50%.
= + 80 (c = 0.5, CH2Cl2).
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D
(3R,8aR)-7-[(1R)-2-(1H-Indol-3-yl)-1-methoxycarbonylethyl]-3-phenyltetrahydrothiazolo[3,4-a]-
pyrazine-5,8-dione (4d) was obtained as a solid (51%). mp 179.9-180.8 °C (from ethyl acetate-hexane).
IR (KBr) 1680, 1735 and 3386 cm-1; 1H NMR δ: 3.08 (1H, dd, J = 12.0 and J = 14.8 Hz), 3.21-3.28 (2H,
m), 3.48 (1H, dd, J = 4.8 and J = 14.8 Hz), 3.81 (3H, s), 3.88 (1H, d, J = 16.9 Hz), 4.10 (1H, d, J = 16.9
Hz), 4.57 (1H, ddd, J = 0.8, J = 6.7 and J = 10.0 Hz), 5.43 (1H, dd, J = 4.8 and J = 12.0 Hz), 6.11 (1H, s),
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6.81-6.83 (2H, m, Ar-H), 7.18-7.29 (8H, m, Ar-H); C NMR δ: 29.6, 30.3, 49.2, 52.7, 56.4, 63.6, 64.2,
109.3, 111.4, 118.3, 119.8, 122.3, 122.9, 124.8, 126.7, 127.8, 128.6, 136.2, 141.1, 163.8, 167.3, 170.5;
MS (ES) m/z 450 (MH+, 100%), 390 (29), 217 (17), 202 (12). Anal. Calcd for C24H23N3O4S: C, 64.13; H,
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5.16; N, 9.35. Found: C, 64.27; H, 4.92; N, 9.13%.
= − 15 (c = 1, CH2Cl2).
[!]
D