1031
121.8, 122.46, 129.18, 130.87, 137.8, 149.1, 153.7,
156.5, 164.6, 171.7.
4b: amorphous, yield: 1.14 g, 44%. Elemental anal. for
C24H31N5O6S (C, H, N, S). H-NMR (DMSO): 2.37 s
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(3H, Me-N), 2.46 s (3H, MsOH), 2.73 t (2H, J = 5.58
Hz), 2.85 t (2H, J = 5.53 Hz), 3.32 m (6H), 3.64 m (2H),
7.19 d (2H, J = 7.45 Hz), 7.36 d (2H, J = 8.24 Hz), 7.45
d (2H, J = 7.46 Hz), 8.17 d (2H, J = 8.22 Hz). 13C-NMR
(DMSO): 29.9 (CH2), 33.6 (CH2), 39.3 (MsOH), 43.1
(MeN), 44.1, 52.9, 53.1, 121.5, 122.5, 122.7, 125.3,
129.5, 138.1, 148.7, 155.5, 164.1, 170.1.
2e: amorphous, yield: 1.17 g, 45%. Elemental anal. for
C24H28N4O9S (C, H, N, S) % S calc. 5.84, found 5.41.
1H-NMR (DMSO): 2.44 (3H, mesylate), 3.45 m (8H),
5.05 s (1H), 7.2–7.32 m (5H), 7.51–7.53 m (2H),
7.77–7.79 m (1H), 8.64 m (1H). 13C-NMR (DMSO):
38.9 (mesylate), 40.7, 43.7, 60.4 (OCH2), 66.3, 118.3,
119.2, 124.6, 126.2, 126.9, 129.5, 129.9, 130.5, 131.6,
133.7, 136.48, 143.8, 146.3, 155.8, 165.8, 1265.9, 167.4.
2f: amorphous, yield: 1.19 g, 45%. Elemental anal. for
4c: amorphous, yield: 1.17 g, 44%. Elemental anal. for
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C24H31N4O8S (C, H, N, S). H-NMR (DMSO): 2.38 s
1
(3H, MsOH), 2.56 t (2H, J = 5.87 Hz), 2.89 t (2H, J =
5.88 Hz), 3.28 bs (2H), 3.87 m (6H), 4.22 d (2H,
CH2NH), 6.66 bs (1H, NH), 6.87 d (2H, J = 7.81 Hz, 7.12
d (2H, J = 7.56 Hz), 7.87 d (2H, J = 7.87 Hz), 7.99 d (2H,
J = 7.53 Hz), 10.11 bs (2H, NH), 11.1 bs (1.5H, NH).
13C-NMR (DMSO): 30.1 (CH2), 31.7 (CH2), 38.9
(MsOH), 40.0, 45.7, 50.2, 53.3, 61.1 (OCH2), 120.1,
122.21, 123.1, 123.8, 125.7, 126.6, 129.3, 138.3, 141.5,
151.3, 158.7, 161.6, 170.0.
C21H25N5O9S (C, H, N, S). H-NMR (DMSO): 2.36 s
(3H, mesylate), 3.55–3.74 2×d (8H), 5.05 s (2H), 6.57 d
(1H), 7.36 d (2H, J = 8.76 Hz), 7.65 d (2H, J = 8.77 Hz),
8.04 dd (1H), 8.29 d (1H). 13C-NMR (DMSO): 39.5
(mesylate), 43.43, 46.15, 62.68 (OCH2), 67.5, 67.6,
111.3, 120.4, 121.5, 124.3, 130.34, 131.3, 135.4, 141.8,
141.9, 155.7, 160.3, 165.8, 174.6.
2g: amorphous, yield: 1.03 g, 39%. Elemental anal. for
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C25H29N3O9S (C, H, N, S). H-NMR, (DMSO): 1.49 s
4d: amorphous, yield: 0.88 g, 38%. Elemental anal. for
C20H26N4O7S (C, H, N, S), % S calc. 6.87, found 6.45.
1H-NMR (DMSO): 2.38 s (3H, MsOH), 3.60 m (8H),
6.67 d (1H, J = 10.26 Hz), 7.23 d (2H, J = 7.83 Hz), 7.36
d (2H, J = 7.22 Hz), 7.66 d (1H, J = 10.3 Hz), 8.06 d (2H,
J = 7.28 Hz), 8.11 d (2H, J = 7.81 Hz). 13C-NMR
(DMSO): 39.91 (MsOH), 42.5, 45.7, 66.2, 66.3, 118.13,
122.3, 122.5, 122.7, 122.8, 129.3, 131.4, 132.9, 140.7,
147.1, 151.6, 154.7, 164.1, 164.5.
(9H, tBuO), 2.46 (3H, mesylate), 4.66 s (2H, OCH2),
6.69 d (1H, J = 11.35 Hz, CH=), 7.19 d (2H, J = 7.45 Hz),
7.45 d (2H, J = 8.1 Hz), 7.71 d (1H, J = 11.36 Hz), 7.89
d (2H, J = 7.98 Hz), 8.17 d (2H, J = 7.44 Hz). 13C-NMR
(DMSO): 27.65, 39.65 (MsOH), 61.14 (OCH2), 81.58,
117.3, 122.43, 122.6, 124.7, 130.5, 131.5, 131.9, 142.1,
143.3, 152.2, 155.6, 163.8, 165.6, 166.8.
2h: amorphous, yield: 1.12 g, 40%. Elemental anal. for
C25H30N4O9S (C, H, N, S) % S calc. 5.70, found 5.39.
1H-NMR (DMSO): 1.42 s (9H, tBuO), 2.38 s (3H,
MsOH), 4.58 s (2H, OCH2), 6.90 d (2H, J = 7.34 Hz),
7.12 dd (1H), 7.36–7.40 m (2H), 7.86 d (2H, J = 7.83
Hz), 8.88 s (1H, NH ind.). 13C-NMR (DMSO): 27.5
(tBu), 36.6 (MsOH), 37.2 (CH2Ar), 56.6 (OCH2), 111.1,
118.69, 119.3, 121.6, 121.8, 121.9, 123.5, 123.9, 125.8,
131.6, 136.3, 141.4, 142.3, 155.1, 161.3, 163.8, 170.9.
2l: amorphous, yield: 1.29 g, 48%. Elemental anal. for
4e: amorphous, yield: 1.22 g, 48%. Elemental anal. for
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C25H26N4O6S (C, H, N, S). H-NMR (DMSO): 2.39 s
(3H, MsOH), 2.75 s (2H, CH2NH), 6.72 d (1H, J = 10.3
Hz), 7.27 m (5H), 7.62 d (2H, J = 7.80 Hz), 7.71 d (2H,
J = 7.21 Hz), 8.08 d (1H, J = 10.4 Hz), 8.17 d (1H, J =
7.85 Hz), 8.24 d, (2H, J = 7.23 Hz). 13C-NMR (DMSO):
39.5 (MsOH), 44.37, 116.7, 122.1, 122.3, 123.3, 123.4,
125.1, 128.3, 128.44, 129.3, 129.8, 130.2, 140.9, 145.3,
155.8, 168.8, 178.2.
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C22H26N4O8S2 (C, H, N, S). H-NMR (DMSO): 2.34 s
(3H, MsOH), 3.56 m (2H), 3.87 m (6H), 7.23 d (2H, J =
7.56 Hz), 7.36 d (2H, J = 7.80 Hz), 7.85 d (2H, J = 7.55
Hz), 7.98 d (2H, J = 7.58 Hz). 13C-NMR (DMSO): 36.7
(MsOH), 45.5, 46.1, 59.1 (OCH2), 65.5, 116.3, 117.5,
117.9, 118.0, 118.2, 121.3, 138.3, 139.8, 155.8, 160.2,
162.1, 165.3.
7a: amorphous, yield: 1.28 g, 49%. Elemental anal. for
C22H27N5O8S (C, H, N, S). H-NMR (DMSO): 2.41 s
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(3H, MsOH), 3.48 m (2H), 3.46 m (6H), 5.62 d (2H,
CH2NH), 7.11 d (2H, J = 7.77 Hz), 7.49 d (2H, J = 7.42
Hz), 7.58 d (2H, J = 7.77 Hz), 8.11 d (2H, J = 7.39 Hz).
13C-NMR (DMSO): 33.3 (MsOH), 40.1, 41.8, 47.5,
(NHCH2), 66.1, 114.8, 122.7, 124.8, 129.1, 131.5, 141.3,
148.5, 155.4, 160.2, 165.1, 167.9.
4a: amorphous, yield: 1.19 g, 46%. Elemental anal. for
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C24H28N4O7S (C, H, N, S). H-NMR (DMSO): 2.36 s
(3H, MsOH), 2.64 t (2H, J = 8.96 Hz), 2.86 t (2H, J =
7.77 Hz), 3.43 m (8H), 7.11 d (2H, J = 6.98 Hz), 7.17 d
(2H, J = 7.85 Hz), 7.37 d (2H, J = 7.00 Hz), 8.04 d (2H,
J = 7.85 Hz). 13C-NMR (DMSO): 33.3 (CH2), 33.7 (CH2),
39.7 (MsOH), 40.4, 66.1 (OCH2), 121.6, 122.0, 122.7,
129.4, 131.2, 138.9, 148.9, 149.5, 154.4, 164.2, 170.0.
7b: amorphous, yield: 1.00 g, 38%. Elemental anal. for
C21H26N4O8S2 (C, H, N, S). H-NMR (DMSO): 2.41 s
(3H, MsOH), 3.40 m (2H), 3.57 m (6H), 4.14 s (2H,
SCH2), 7.39 d (2H, J = 7.33 Hz), 7.59 d (2H, J = 7.87
Hz), 8.05 d (2H, J = 7.34 Hz), 8.19 d (2H, J = 7.87 Hz).
13C-NMR (DMSO): 39.5 (MsOH), 42.1, 45.9, 52.7
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