第三章 實驗部分
3.7 Synthesis of Pyrrole II-48
(Z)-3-(4-Phenyl-1-tosyl-1H-pyrrol-3-yl)-1-(p-tolyl)prop-2-en-1-one (II-48a)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47a (0.110 g, 0.25 mmol) in 1.5 mL toluene, after 5 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:30) to give product II-48a as a yellow oil (0.071 g, 0.16 mmol, 62%) : Rf 0.35 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.54 (d, J = 2.1 Hz, 1H), 7.88 (d, J = 8.1 Hz, 2H), 7.84 (d, J = 8.2 Hz, 2H), 7.42 – 7.37 (m, 2H), 7.36 – 7.28 (m, 5H), 7.26 – 7.22 (m, 2H), 7.18 (d, J = 2.3 Hz, 1H), 6.79 (s, 2H), 2.41 (s, 3H), 2.40 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 191.0, 145.3, 143.4, 136.0, 135.6, 133.0, 132.9, 131.1, 130.1, 129.2, 129.1, 129.0, 127.4, 127.2, 124.7, 122.6, 121.5, 117.7, 21.6 ppm.IR (CH
2Cl2): ν 2360, 1656, 1607, 1441, 1375, 1231, 1174, 1066, 670, 584 cm-1.MS (ESI) m/e (%) 442.5 ([M+H]
+, 100), 464.5 ([M+Na]+, 65)HRMS (ESI) m/e calcd for C
27H24NO3S [M+H]+ 442.1477, found 442.1477.- 89 -
(Z)-1-(3-Methoxyphenyl)-3-(4-phenyl-1-tosyl-1H-pyrrol-3-yl)prop-2-en-1-
one (II-48b)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47b (0.114 g, 0.25 mmol) in 1.5 mL toluene, after 8 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:27) to give product II-48b as a yellow oil (0.081 g, 0.18 mmol, 70%) : Rf 0.25 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.56 (d, J = 2.4 Hz, 1H), 7.84 (d, J = 8.3 Hz, 2H), 7.56 – 7.50 (m, 2H), 7.43 – 7.37 (m, 2H), 7.37 – 7.28 (m, 6H), 7.19 (d, J = 2.3 Hz, 1H), 7.09 (dd, J = 8.2, 2.6 Hz, 1H), 6.80 (s, 2H), 3.88 (s, 3H), 2.40 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 191.0, 159.9, 145.3, 140.0, 135.7, 133.5, 133.0, 131.2, 130.1, 129.5, 129.2, 128.6, 127.5, 127.3, 124.8, 122.4, 121.5, 121.1, 119.3, 117.7, 112.6, 55.5, 21.7 ppm.IR (CH
2Cl2): ν 2930, 1659, 1590, 1438, 1377, 1264, 1174, 1067, 671, 584 cm-1.MS (ESI) m/e (%) 480.3 ([M+Na]
+, 100), 458.4 ([M+H]+, 28)HRMS (ESI) m/e calcd for C
27H24NO4S [M+H]+ 458.1426, found 458.1427.- 90 -
(Z)-1-(4-Methoxyphenyl)-3-(4-phenyl-1-tosyl-1H-pyrrol-3-yl)prop-2-en-1-
one (II-48c)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47c (0.114 g, 0.25 mmol) in 1.5 mL toluene, after 25 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:35) to give product II-48c as a yellow oil (0.093 g, 0.21 mmol, 82%) : Rf 0.18 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 7.89 – 7.80 (m, 4H), 7.70 – 7.62 (m, 1H), 7.60 (d, J = 2.3 Hz, 1H), 7.44 – 7.38 (m, 2H), 7.38 – 7.31 (m, 5H), 7.25 – 7.18 (m, 2H), 6.95 – 6.89 (m, 2H), 3.87 (s, 3H), 2.43 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 188.1, 163.3, 145.7, 135.4, 135.2, 133.0, 130.9, 130.6, 130.3, 129.9, 128.9, 128.7, 127.6, 127.2, 123.8, 122.1, 121.0, 119.2, 113.7, 55.5, 21.7 ppm.IR (CH
2Cl2): ν 1655, 1602, 1372, 1260, 1172, 1070, 808, 734, 671, 587 cm-1.MS (ESI) m/e (%) 458.2 ([M+H]
+, 100), 460.2 ([M+2+H] +, 29).HRMS (ESI) m/e calcd for C
27H24NO4S [M+H]+ 458.1426, found 458.1426.- 91 -
(Z)-5-Phenyl-1-(4-phenyl-1-tosyl-1H-pyrrol-3-yl)pent-1-en-4-yn-3-one (II-48d)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47d (0.113 g, 0.25 mmol) in 1.5 mL toluene, after 50 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:35) to give product II-48d as a yellow oil (0.079 g, 0.18 mmol, 71%) : Rf 0.20 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.69 (d, J = 2.1 Hz, 1H), 7.90 – 7.85 (m, 2H), 7.54 – 7.49 (m, 2H), 7.46 – 7.26 (m, 10H), 7.23 (d, J = 2.4 Hz, 1H), 6.74 (dd, J= 12.4, 0.6 Hz, 1H), 6.41 (d, J = 12.4 Hz, 1H), 2.38 (s, 3H) ppm.
13
C NMR (100 MHz, CDCl
3): δ 175.7, 145.5, 135.5, 134.9, 133.0, 132.8, 131.1, 130.5, 130.2, 129.2, 128.6, 128.5, 127.6, 127.3, 126.0, 125.8, 121.4, 120.3, 117.8, 90.4, 89.9, 21.7 ppm.IR (CH
2Cl2): ν 2203, 1641, 1587, 1430, 1377, 1172, 1064, 811, 756, 670, 583 cm-1.MS (ESI) m/e (%) 452.2 ([M+H]
+, 100), 454.2 ([M+2+H] +, 30).HRMS (ESI) m/e calcd for C
28H22NO3S [M+H]+ 452.1320, found 452.1326.- 92 -
(Z)-1-(4-Phenyl-1-tosyl-1H-pyrrol-3-yl)-5-(o-tolyl)pent-1-en-4-yn-3-one (II-48e)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47e (0.116 g, 0.25 mmol) in 1.5 mL toluene, after 10 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:60) to give product II-48e as a yellow oil (0.079 g, 0.17 mmol, 68%) : Rf 0.30 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.72 (d, J = 2.2 Hz, 1H), 7.90 – 7.85 (m, 2H), 7.49 (dd, J = 7.6, 0.9 Hz, 1H), 7.43 – 7.37 (m, 2H), 7.37 – 7.33 (m, 1H), 7.33 – 7.28 (m, 4H), 7.28 – 7.26 (m, 1H), 7.25 – 7.20 (m, 2H), 7.20 – 7.14 (m, 1H), 6.73 (d, J = 12.4 Hz, 1H), 6.41 (d, J = 12.5 Hz, 1H), 2.44 (s, 3H), 2.38 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 175.8, 145.5, 142.2, 135.5, 134.6, 133.5, 132.8, 131.2, 130.6, 130.2, 129.7, 129.2, 128.6, 127.6, 127.3, 126.1, 125.8, 125.7, 121.3, 120.1, 117.8, 94.4, 89.0, 21.7, 20.6 ppm.IR (CH
2Cl2): ν 2933, 2182, 1638, 1602, 1508, 1430, 1376, 1170, 1062, 834, 671, 587 cm-1.MS (ESI) m/e (%) 518.5 ([M+Na]
+, 100), 520.5 ([M+2+Na] +, 29).HRMS (ESI) m/e calcd for C
30H26NO4S [M+H]+ 496.1583, found 496.1581.- 93 -
(Z)-1-(4-Phenyl-1-tosyl-1H-pyrrol-3-yl)-5-(m-tolyl)pent-1-en-4-yn-3-one (II-48f)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47f (0.116 g, 0.25 mmol) in 1.5 mL toluene, after 15 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:40) to give product II-48f as a yellow oil (0.066 g, 0.14 mmol, 57%) : Rf 0.30 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.68 (d, J = 2.1 Hz, 1H), 7.87 (d, J = 8.3 Hz, 2H), 7.43 – 7.32 (m, 4H), 7.32 – 7.26 (m, 5H), 7.25 – 7.21 (m, 3H), 6.73 (d, J = 12.5 Hz, 1H), 6.40 (d, J = 12.4 Hz, 1H), 2.38 (s, 3H), 2.33 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 175.8, 145.5, 138.3, 135.5, 134.8, 133.6, 132.8, 131.4, 131.1, 130.2, 129.2, 128.6, 128.4, 127.5, 127.3, 126.0, 125.9, 121.4, 120.1, 117.7, 90.4, 90.2, 21.7, 21.1 ppm.IR (CH
2Cl2): ν 2923, 2192, 1640, 1589, 1431, 1377, 1177, 1066, 757, 672, 585 cm-1.MS (ESI) m/e (%) 488.3 ([M+Na]
+, 100), 466.4 ([M+H] +, 27).HRMS (ESI) m/e calcd for C
29H24NO3S [M+H]+ 466.1477, found 466.1478.- 94 -
(Z)-1-(4-Phenyl-1-tosyl-1H-pyrrol-3-yl)-5-(p-tolyl)pent-1-en-4-yn-3-one (II-48g)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47g (0.116 g, 0.25 mmol) in 1.5 mL toluene, after 10 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:35) to give product II-48g as a yellow oil (0.093 g, 0.20 mmol, 80%) : Rf 0.35 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.68 (d, J = 2.3 Hz, 1H), 7.87 (d, J = 8.4 Hz, 2H), 7.43 – 7.37 (m, 4H), 7.37 – 7.26 (m, 5H), 7.23 (d, J = 2.3 Hz, 1H), 7.16 (d,J = 8.0 Hz, 2H), 6.72 (d, J = 12.4 Hz, 1H), 6.39 (d, J = 12.5 Hz, 1H), 2.38 (s,
6H) ppm.
13
C NMR (100 MHz, CDCl
3): δ 175.8, 145.5, 141.2, 135.5, 134.6, 133.1, 132.8, 131.1, 130.2, 129.4, 129.2, 128.6, 127.5, 127.3, 126.0, 121.4, 117.7, 117.2, 90.7, 90.3, 21.7, 21.6 ppm.IR (CH
2Cl2): ν 2202, 1639, 1430, 1376, 1172, 1064, 816, 670, 586 cm-1.MS (ESI) m/e (%) 488.3 ([M+Na]
+, 100), 466.4 ([M+H] +, 16).HRMS (ESI) m/e calcd for C
29H24NO3S [M+H]+ 466.1477, found 466.1481.- 95 -
(Z)-5-(4-Methoxyphenyl)-1-(4-phenyl-1-tosyl-1H-pyrrol-3-yl)pent-1-en-4-
yn-3-one (II-48h)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47h (0.120 g, 0.25 mmol) in 1.5 mL toluene, after 10 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:35) to give product II-48h as a yellow oil (0.084 g, 0.18 mmol, 70%) : Rf 0.23 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.66 (d, J = 2.4 Hz, 1H), 7.90 – 7.84 (m, 2H), 7.49 – 7.43 (m, 2H), 7.43 – 7.37 (m, 2H), 7.37 – 7.26 (m, 5H), 7.23 (d, J = 2.4 Hz, 1H), 6.89 – 6.83 (m, 2H), 6.71 (dd, J = 12.4, 0.5 Hz, 1H), 6.39 (d, J = 12.4 Hz, 1H), 3.84 (s, 3H), 2.38 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 175.9, 161.5, 145.4, 135.5, 135.1, 134.4, 132.8, 131.0, 130.2, 129.2, 128.6, 127.5, 127.3, 126.1, 125.9, 121.4, 117.7, 114.3, 112.1, 91.2, 90.3, 55.4, 21.7 ppm.IR (CH
2Cl2): ν 2923, 2183, 1601, 1508, 1377, 1253, 1171, 1064, 671, 587 cm-1.MS (ESI) m/e (%) 504.3 ([M+Na]
+, 100), 482.4 ([M+H] +, 34).HRMS (ESI) m/e calcd for C
29H24NO4S [M+H]+ 482.1426, found 482.1426.- 96 -
(Z)-5-([1,1'-Biphenyl]-4-yl)-1-(4-phenyl-1-tosyl-1H-pyrrol-3-yl)pent-1-en-4 -yn-3-one (II-48i)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47i (0.132 g, 0.25 mmol) in 1.5 mL toluene, after 18 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:50) to give product II-48i as a yellow oil (0.075 g, 0.14 mmol, 57%) : Rf 0.33 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.69 (d, J = 2.1 Hz, 1H), 7.91 – 7.85 (m, 2H), 7.62 – 7.56 (m, 6H), 7.49 – 7.44 (m, 2H), 7.43 – 7.34 (m, 4H), 7.34 – 7.30 (m, 2H), 7.28 (d, J = 8.2 Hz, 2H), 7.24 (d, J = 2.3 Hz, 1H), 6.76 (dd, J = 12.4, 0.7 Hz, 1H), 6.42 (d, J = 12.4 Hz, 1H), 2.37 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 175.7, 145.5, 143.3, 139.8, 135.5, 134.9, 133.6, 132.8, 131.1, 130.2, 129.2, 129.0, 128.7, 128.1, 127.6, 127.4, 127.2, 127.1, 126.0, 125.9, 121.4, 119.0, 117.8, 91.1, 90.0, 21.7 ppm.IR (CH
2Cl2): ν 2927, 2200, 1638, 1589, 1377, 1172, 1064, 671, 585 cm-1.MS (ESI) m/e (%) 550.4 ([M+Na]
+, 100), 552.4 ([M+2+Na] +, 34).HRMS (ESI) m/e calcd for C
34H26NO3S [M+H]+ 528.1633, found 528.1633.- 97 -
(Z)-5-(3-Nitrophenyl)-1-(4-phenyl-1-tosyl-1H-pyrrol-3-yl)pent-1-en-4-yn-3-one (II-48j)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47j (0.124 g, 0.25 mmol) in 1.5 mL toluene, after 10 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:20) to give product II-48j as a yellow oil (0.103 g, 0.21 mmol, 83%) : Rf 0.18 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.67 (d, J = 2.1 Hz, 1H), 8.31 (t, J = 1.8 Hz, 1H), 8.27 (ddd, J = 8.3, 2.3, 1.1 Hz, 1H), 7.91 – 7.86 (m, 2H), 8.32 (dt, J = 7.7, 1.2 Hz, 1H), 7.57 (t, J = 8.1 Hz, 1H), 7.43 – 7.38 (m, 2H), 7.38 – 7.34 (m, 1H), 7.34 – 7.28 (m, 4H), 7.26 – 7.25 (m, 1H), 6.83 (d, J = 12.2 Hz, 1H), 6.41 (d, J= 12.4 Hz, 1H), 2.39 (s, 3H) ppm.
13
C NMR (100 MHz, CDCl
3): δ 174.9, 148.1, 145.6, 138.3, 136.2, 135.4, 132.6, 131.1, 130.2, 129.7, 129.1, 128.7, 127.7, 127.6, 127.4, 126.2, 125.3, 124.9, 122.2, 121.3, 117.9, 91.3, 85.9, 21.7 ppm.IR (CH
2Cl2): ν 2207, 1643, 1532, 1377, 1353, 1173, 1065, 811, 670, 584 cm-1.MS (ESI) m/e (%) 519.6 ([M+Na]
+, 60).HRMS (ESI) m/e calcd for C
28H21N2O5S [M+H]+ 497.1171, found 497.1169.- 98 -
(Z)-1-(4-Phenyl-1-tosyl-1H-pyrrol-3-yl)-5-(thiophen-3-yl)pent-1-en-4-yn-3-one (II-48k)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47k (0.114 g, 0.25 mmol) in 1.5 mL toluene, after 8 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:45) to give product II-48k as a yellow oil (0.066 g, 0.15 mmol, 58%) : Rf 0.33 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.66 (d, J = 2.3 Hz, 1H), 7.87 (d, J = 8.4 Hz, 2H), 7.66 (dd, J = 2.9, 1.0 Hz, 1H), 7.43 – 7.37 (m, 2H), 7.37 – 7.33 (m, 1H), 7.33 – 7.27 (m, 5H), 7.23 (d, J = 2.4 Hz, 1H), 7.16 (dd, J = 5.0, 0.8 Hz, 1H), 6.74 (d, J = 12.4 Hz, 1H), 6.38 (d, J = 12.4 Hz, 1H), 2.39 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 175.7, 145.5, 135.4, 134.9, 133.6, 132.7, 131.0, 130.3, 130.2, 129.1, 128.6, 127.6, 127.3, 126.0, 125.9, 125.8, 121.4, 119.6, 117.7, 90.5, 85.3, 21.7 ppm.IR (CH
2Cl2): ν 2922, 2198, 1638, 1588, 1432, 1377, 1172, 1064, 671, 585 cm-1.MS (ESI) m/e (%) 480.5 ([M+Na]
+, 100), 482.5 ([M+2+Na] +, 25).HRMS (ESI) m/e calcd for C
26H20NO3S2 [M+H]+ 458.0885, found 458.0886.- 99 -
Methyl (Z)-3-(3-oxo-5-(4-phenyl-1-tosyl-1H-pyrrol-3-yl)pent-4-en-1-yn-1- yl)benzoate (II-48l)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47l (0.127 g, 0.25 mmol) in 1.5 mL toluene, after 20 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:15) to give product II-48l as a yellow oil (0.090 g, 0.18 mmol, 71%) : Rf 0.23 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.67 (d, J = 2.1 Hz, 1H), 8.16 (t, J = 1.4 Hz, 1H), 8.08 (dt, J = 7.9, 1.5 Hz, 1H), 7.90 – 7.85 (m, 2H), 7.68 (dt, J = 7.7, 1.4 Hz, 1H), 7.48 – 7.38 (m, 3H), 7.37 – 7.30 (m, 3H), 7.28 (d, J = 8.0 Hz, 2H), 7.24 (d, J = 2.4 Hz, 1H), 6.78 (dd, J = 12.6, 0.6 Hz, 1H), 6.41 (d, J = 12.4 Hz, 1H), 3.93 (s, 3H), 2.38 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 175.4, 165.9, 145.5, 136.9, 135.5, 134.1, 132.7, 131.3, 131.0, 130.7, 130.2, 129.1, 128.8, 128.7, 127.6, 127.4, 126.1, 125.7, 121.4, 120.8, 117.8, 90.6, 88.3, 52.4, 21.7 ppm.IR (CH
2Cl2): ν 2923, 2238, 1600, 1514, 1333, 1169, 1020, 753, 691, 573 cm-1.MS (ESI) m/e (%) 532.4 ([M+Na]
+, 100), 534.4 ([M+2+Na] +, 28).HRMS (ESI) m/e calcd for C
30H24NO5S [M+H]+ 510.1375, found 510.1376.- 100 -
(Z)-5-(4-Methoxyphenyl)-1-(4-(o-tolyl)-1-tosyl-1H-pyrrol-3-yl)pent-1-en-4-yn-3-one (II-48m)
According to GP 2-6, AuCl3 (0.0038 g, 0.0125 mmol), dry toluene (1.0 mL), II-47m (0.124 g, 0.25 mmol) in 1.5 mL toluene, after 30 min, product was obtained. The crude mixture was purified via flash column chromatography over silica gel (EtOAc/hexanes 1:27) to give product II-48m as a yellow oil (0.079 g, 0.16 mmol, 64%) : Rf 0.23 (EtOAc/hexanes 1:5).
1
H NMR (400 MHz, CDCl
3): δ 8.86 (d, J = 2.3 Hz, 1H), 7.88 (d, J = 8.4 Hz, 2H), 7.53 – 7.46 (m, 2H), 7.31 (d, J = 8.2 Hz, 2H), 7.29 – 7.25 (m, 2H), 7.19 (td, J = 7.0, 2.3 Hz, 1H), 7.14 – 7.08 (m, 2H), 6.91 – 6.84 (m, 2H), 6.34 – 6.25 (m, 2H), 3.84 (s, 3H), 2.41 (s, 3H), 2.12 (s, 3H) ppm.13
C NMR (100 MHz, CDCl
3): δ 175.6, 161.5, 145.4, 137.4, 135.6, 135.0, 134.3, 132.0, 131.1, 130.4, 130.2, 128.1, 127.3, 125.8, 125.6, 125.1, 122.6, 118.3, 114.3, 112.1, 90.9, 90.5, 55.4, 21.7, 20.3 ppm.IR (CH
2Cl2): ν 2923, 2238, 1600, 1514, 1333, 1169, 1020, 753, 691, 573 cm-1.MS (ESI) m/e (%) 532.4 ([M+Na]
+, 100), 534.4 ([M+2+Na] +, 28).HRMS (ESI) m/e calcd for C
30H24NO5S [M+H]+ 510.1375, found 510.1376.- 101 -
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