Journal of Sulfur Chemistry 455
121.8, 116.4, 115.7, 86.3, 70.8, 43.11, 21.2. Anal. calcd for C20H16N4OS: C 66.64, H 4.47, N
15.54. Found C 66. 59, H 4.51, N 15.48.MS (EI) (m/z): 360 (M+).
4.5. 2,4-Diamino-5(benzylthio)-5H-chromeno[2,3-b]pyridine-3-carbonitrile(3a)
Yellow solid, IR (KBr) (vmax/cm−1): 3377, 3439, 2200, 1400, 1605; 1H NMR (400 MHz, DMSO-
d6): δ = 3.49 (ABq, 2H, J = 12 Hz), 5.48 (1H), 6.55 (bs, 2H), 6.83 (bs, 2H), 7.03–7.21 (m, 7H),
7.33 (m, 2H); 13C NMR (100 MHz, DMSO-d6): δ = 160.2, 159.9, 152.9, 143.7, 136.6, 133.3,
133.2, 129.6, 129.4, 124.3, 124.2,122.8, 119.3, 118.3, 117.6, 87.01, 70.90, 44.01, 37.02. Anal.
calcd for C20H16N4OS: C 66.64, H 4.47, N 15.54. Found C 66. 48, H 4.58, N 15.39.MS (EI)
(m/z): 360 (M+).
4.6. 5-((Furan-2-yl) methylthio)-2,4-diamino-5H-chromeno[2,3-b]pyridine-3-carbonitrile
(4a)
Yellow solid, IR (KBr) (vmax/cm−1): 3386, 3440, 2203, 1397, 1612;1H NMR (400 MHz, DMSO-
d6): δ = 3.51 (ABq, 2H, J = 12 Hz), 5.46(1H), 5.99 (1H), 6.23 (s, 1H), 6.55 (bs, 2H), 6.79 (bs,
2H), 7.10(d, 1H, J = 8 Hz), 7.17 (t, 1H, J = 8 Hz), 7.24(s, 1H), 7.31(t, 2H, J = 8 Hz); 13C NMR
(100 MHz, DMSO-d6): δ = 160.10, 160.3, 157.1, 151.2, 149.4, 142.7, 133.8, 129.7, 129.0, 116.9,
116.5, 111.0, 107.8, 87.9, 71.0, 35.03, 25.9. Anal. calcd for C18H14N4O2S: C 61.70, H 4.03, N
15.99. Found C 61.62, H 4.10, N 15.91. MS (EI) (m/z): 350(M+).
4.7. 2,4-Diamino-5-(benzylthio)-7-bromo-5H-chromeno[2,3-b]pyridine-3-carbonitrile (3b)
Yellow solid, IR (KBr) (vmax/cm−1): 3315, 3441, 2189, 1403, 1653; 1H NMR (400 MHz, DMSO-
d6) δ = 4.06–4.45 (ABq, 2H, J = 12 Hz), 4.67 (1H), 6.48 (s, 1H), 6.88–6.90 (m, 5H), 7.37 (m,6H);
13C NMR (100 MHz, DMSO-d6) δ = 160.80, 160.44, 152.75, 148.22, 137.96, 137.53, 131.05,
129.79, 128.60, 124.41,121.60, 120.90, 118.79, 116.46, 87.22, 35.78, 35.4, 33.34. Anal. calcd
for C20H15N4OSBr: C 54.68, H 3.44, N 12.75. Found C 54.55, H 3.52, N 12.61. MS (EI) (m/z):
439(M+).
4.8. 5-((Furan-2-yl)methylthio)-2,4-diamino-7-bromo-5H-chromeno[2,3-b]pyridine-3-
carbonitrile (4b)
Yellow solid, IR (KBr) (vmax/cm−1):3311, 3442, 2194, 1404, 1655;1H NMR (400 MHz, DMSO-
d6) δ = 4.14–4.56 (ABq, 2H, J = 12 Hz), 4.89 (1H), 6.34 (s, 1H), 6.46 (d, J = 8.3 Hz,1H),
6.78–6.95 (m, 6H), 7.39 (d, 1H, J = 9 Hz), 7.62 (d, 1H);13C NMR (100 MHz, DMSO-d6) δ =
160.5, 155.24, 150.72, 148.21, 143.26, 131.89, 131.12, 125.50, 124.14, 119.41, 118.87, 116.50,
111.49, 108.77, 84.86, 54.27, 36.31, 28.64. Anal. calcd for C18H13N4O2SBr: C 50.39, H 3.05, N
13.06. Found C 50.35, H 2.97, N 13.01.MS (EI) (m/z): 429 (M+).
4.9. Catalyst recovery
In the recycling procedure of ZrP2O7 NPs, DMF was added to dilute the reaction mixture after
terminating the reaction. The catalyst was insoluble in the solvent and was separated by simple
filtration. The recovered ZrP2O7 NPs was washed with ethanol and dried at 70◦C for 2 h. The
separated catalyst was used several times with a slightly decreased activity as given in Table 3.