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CAS No. : | 1370206-12-4 | MDL No. : | N/A |
Formula : | C22H15N3O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | WLMLPFKCGMQBFL-UHFFFAOYSA-N |
M.W : | 353.37 | Pubchem ID : | 102289736 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P301+P312-P302+P352-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
39% | With sodium hydroxide; In water; at 170.0℃; for 72.25h;pH 2.0;Autoclave; | A mixture of Cu(NO3)2·3H2O (0.4 mmol), H3btc (0.2 mmol), Htpba (0.2 mmol), NaOH (0.3 mmol) and distilled water (8 mL) was stirred for 15 min in air (solution pH= 2.0), then transferred and sealed in an 18 mL Teflon-lined autoclave, which was heated at 170 C for 72 h. After slow cooling to room temperature, green block crystals of 1 were filtered off, washed with distilled water, and dried at ambient temperature (yield: 39 % based on Cu). Elemental analysis (%) calcd for C31H22N3O9.5Cu: C 57.10, H 3.40, N 6.44, Cu 9.75; found: C 56.94, H 3.61, N 6.27, Cu 9.93 %. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
30% | at 100.0℃; for 72h;High pressure; | Both complexes were prepared by hydro(solvo)thermal reactions. A mixture of MnCl2·4H2O (0.1mmol), 4-Hcptpy (0.05mmol), 5mL DMF and 1mL water was sealed in a 10mL Teflon-lined reactor. The reactor was heated at 100C for 72h. A clear solution without any solid was afforded. Colorless crystals of complex 1 were grown from the solution after one week in 30% yield based on 4-Hcptpy. Anal. Calcd. for C50H46MnN8O8 (%): C, 63.76; H, 4.92; N, 11.90. Found: C, 63.31; H, 4.72; N, 11.32. IR (KBr, cm-1): 3417m, 3074w, 2934w, 1657s, 1595s, 1548s, 1390s, 827s, 788s, 632m. The experimental and simulated PXRD patterns of 1 are in good agreement with each other (Fig. S1, ESI). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With 1,2,4,5-benzenetetracarboxylic acid; In N,N-dimethyl-formamide; at 120.0℃; for 72h;High pressure; | A mixture of Co(NO3)2·6H2O (0.2mmol), 4-Hcptpy (0.1mmol), 1,2,4,5-benzenetetracarboxylic acid (0.1mmol), 2mL DMF and 6mL water was sealed in a 10mL Teflon-lined reactor. The reactor was heated at 120C for 72h, and then cooled to room temperature at a rate of 10Ch-1. Several red crystals of complex 2 were obtained. IR (KBr, cm-1): 3394m, 3068w, 1596s, 1528s, 1391s, 1018m, 842s, 829m, 784s, 694m, 632m. The complex 2 can be prepared with a similar procedure except that 1,2,3,4,5,6-cyclohexanehexacarboxylic acid was used instead of 1,2,4,5-benzenetetracarboxylic acid, but the yield is still poor. It was failed to prepare 2 without the addition of benzenetetracarboxylic acid or cyclohexanehexacarboxylic acid. This indicates that the preparation of 2 may be highly influenced by pH value. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
83% | A mixture of Mptpy (2.16g, 6.7mmol), KMnO4 (4.20g, 26.7mmol), and H2O (100mL) were added to a round bottom flask and stirred at room temperature. In this period, the solution was adjusted to pH=10.0 with the addition of KOH. After stirring for 2h at 100, the mixture was filtered and washed with hot water. And then the filtrate was made slightly acidic (pH=5.0) by the addition of HCl (aq., conc.), the precipitate was filtered off and dried in vacuo to give a white powder. Yield: 1.95g (83%). Anal. Calc. for C22H15O2N3 (Mr =353.11) (%): C, 74.78; H, 4.28; N, 11.89. Found (%): C, 74.23; H, 4.92; N, 11.37. IR(KBr, cm-1): 3407(s), 3090(m), 2024(w), 1693(s), 1631(s), 1600(s), 1506(s), 1425(w), 1397(m), 1328(w), 1119(m), 834(m), 778(m), 617(m). ESI-MS: [M-H]- calcd. for C22H14O2N3: 352.1092; found: 352.1090. 1H NMR (400MHz, (CD3)2SO2) δ: 9.02 (m, 4H), 8.85-8.78 (m, 6H), 8.30 (d, J=8.0, 2H), 8.14 (d, J=8.0, 2H). 13C NMR (100MHz, (CD3)2SO2) δ: 166.87, 152.44, 151.38, 149.91, 143.87, 140.01, 132.10, 129.95, 128.05, 123.93, 122.24. (Figs. S1 and S2, Supporting Information). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
49.2% | With sodium hydroxide; In N,N-dimethyl acetamide; at 180.0℃; for 72h;pH 6.0;High pressure; | Compound 1 was synthesized in a similar procedure as Method 1, by using ZnCl2 (0.0166g, 0.1mmol) in place of Zn(NO3)2·6H2O. The yellow block crystalline product was obtained, washed with distilled water (5mL), and dried in air to give 0.0383g, yield 49.2% based on Zn. Elemental anal. calcd for: C88H56N12Zn2O9 (%):C 67.92, H 3.63, N 10.80; found: C 67.75, H 3.65, N 10.39. IR(KBr, cm-1): 3414(s), 3132(s), 1597(s), 1548(s), 1399(vs), 1221(w), 1138(w), 1066(w), 1021(w), 831(w), 781(m), 700(m), 632(m), 489(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
61.8% | With sodium hydroxide; at 180℃; for 72h;pH 4.5;High pressure; | A mixture of Zn(NO3)2·6H2O (0.0291g, 0.1mmol), Hcptpy (0.0277g, 0.05mmol), and H3idc (0.0126g, 0.1mmol) in distilled water (10mL) that adjusted the pH value to 4.5 with 0.5molL-1 NaOH aqueous solution was placed in a Teflon-lined tainless steel vessel (25mL), heated to 180 for 72h and then cooled to room temperature at a rate of 5/h. The yellow sheet crystalline products of 2 were obtained, washed with distilled water (5mL), and dried in air to give 0.0321g (yield 61.8% based on Zn). Anal. Calc. for C49H31N8Zn2O11 (%): C, 56.67; H, 3.00; N, 10.79. Found: C, 56.52; H, 3.08; N, 10.32%. IR(KBr, cm-1): 3133(s), 1596(m), 1548(m), 1401(vs), 1251(w), 1132(w), 870(w), 829(m), 784(m), 707(m), 634(w), 517(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
69% | In a typical preparation, 4-acetylpyridine (1.21g, 10mmol) was added to a stirred solution of 4-carboxybenzaldehyde (0.75g, 5mmol), KOH (0.8g, 14mmol) and NH3·H2O (20mL) in 150mL ethanol. The reaction mixture was stirred at room temperature whilst open to air for 48h, after which the solution was made slightly acidic (pH=5) with the addition of HCl (aq., conc.). The resulting light yellow precipitate was filtered off, recrystallized with a mixture of ethanol and methanol, and dried in vacuo to give white powders. Yield: 1.22g (69%). ESI-MS: [M-H]- calcd. for C22H14N3O2: 352.1092; found: 352.1090. 1H NMR (400MHz, (CD3)2SO2) δ: 9.02 (m, 4H), 8.85-8.78 (m, 6H), 8.30 (d, J=8.0, 2H), 8.14 (d, J=8.0, 2H). 13C NMR (100MHz, (CD3)2SO2) δ: 166.87, 152.44, 151.38, 149.91, 143.87, 140.01, 132.10, 129.95, 128.05, 123.93, 122.24. (Figs. S1 and S2, supporting information). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62.2% | With sodium hydroxide; In N,N-dimethyl acetamide; at 180.0℃; for 72h;pH 6.0;High pressure; | Compound 1 was prepared by hydrothermal reaction of Zn(NO3)2·6H2O (0.0136g, 0.1mmol) and Hcptpy (0.0277g, 0.1mmol) in distilled water (8mL) and N,N-dimethylacetamide (DMA) (2mL) and using 0.5molL-1 NaOH aqueous solution to adjust the pH to 6.0 that was placed in a Teflon-lined stainless steel vessel (25mL), heated to 180 for 72h and then cooled to room temperature at a rate of 5/h. The yellow block crystalline product was obtained, washed with distilled water (5mL), and dried in air to give 0.0484g, yield 62.2% based on Zn. Elemental anal. calcd for: C88H56N12Zn2O9 (%): C 67.92, H 3.63, N 10.80; found: C 67.75, H 3.65, N 10.39. IR(KBr, cm-1): 3414(s), 3132(s), 1597(s), 1548(s), 1399(vs), 1221(w), 1138(w), 1066(w), 1021(w), 831(w), 781(m), 700(m), 632(m), 489(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | In methanol; at 85.0℃; for 72h;High pressure; | A mixture of Cu(NO3)2·3H2O (20.0mg, 0.08mmol), Hcptpy (15.0mg, 0.04mmol), DMA/MeOH/H2O (2.5mL, v/v/v 3:1:1) and HNO3 (50µL) was placed in a 23mL glass vial and heated at 85C for 3days. The blue crystals were collected and washed with DMF (yield: 65% based on the ligand). Anal. Calc. (Found) for C25H25CuN5O8: C, 51.15 (51.10); H, 4.29 (4.50); N, 11.93 (11.87)%. Selected IR (KBr, cm-1): 3121, 1621, 1602, 1558, 1540, 1520, 1505, 1448, 1398, 1304, 1219, 1187, 1061, 1012, 873, 854, 782, 714, 653. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | In methanol; at 80.0℃; for 72h;Heating; | A mixture of Zn(NO3)2·6H2O (18.0mg, 0.06mmol), Hcptpy (10mg, 0.03mmol), DMA/H2O (2.5mL, v/v 4:1) and HNO3 (50µL) was placed in a 23mL glass vial and heated at 80C for 3days. The pale-yellow crystals were collected and washed with DMF (yield: 40% based on the ligand). Anal. Calc. (Found) for C81H89Zn3N17O26: C, 50.86 (50.76); H, 4.69 (4.54); N, 12.45 (12.37)%. Selected IR (KBr, cm-1): 3373, 1667, 1601, 1548, 1384, 1324, 1261, 1215, 1063, 1022, 840, 786, 710, 649, 619. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In acetonitrile; at 160.0℃; for 75h;Autoclave; | 1) 0.05 mmol of zinc nitrate hexahydrate, 0.05 mmol of Hcptpy and 0.025 mmol of H3btc were added to 2.0 ml of acetonitrile and 4.0 ml of distilled water to obtain a mixed solution;2) The above mixture was transferred to a 25 ml stainless steel autoclave lined with polytetrafluoroethylene, heated to 160 C for 3 hours, held at 160 C for 72 hours, and then cooled to 30 C over 48 hours to obtain a light yellow color. The cluster crystals were washed three times with acetonitrile and water, respectively, and dried to obtain the desired product. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
17.7% | With sodium hydroxide; at 160.0℃; for 72h;pH 6.0; | A mixture of Nd(NO3)3 ·6H2O (0.0439 g, 0.1 mmol), HCptpy (0.0353 g,0.1 mmol), and H2Glu (0.0132 g, 0.1 mmol) in distilledwater (10 mL) that adjusted the pH value to 6.0with 0.5 mol L-1 NaOH aqueous solution was placedin a Teflon-lined stainless steel vessel (25 mL), heatedto 160C for 72 h and then cooled to room temperatureat a rate of 5C/h. The crystalline products of I wereobtained, washed with distilled water (5 mL), anddried in air to give 0.0121 g (yield 17.7% based on Nd).IR (KBr; ν, cm-1): 3587 w, 3418 s, 2975 w, 2353 w,1538 s, 1446 s, 1411 s, 1356 w, 1308 w, 1221 w, 1058 w,880 w, 813 w, 754 w, 660 m. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 150.0℃; for 72.6667h;Autoclave; | For complex 2, we mixed 0.2 mmol 0.027 g ZnCl2,0.25 mmol 0.088 g H1L2, and 5mL of H2O to form a mixtureand kept it in the 25 ml stainless steel container lined withTeflon, stirred it for forty minutes and then heated it for 72 hat 150 . After cooling it to the ambient temperature, we acquiredcolorless crystals with block shape (the yield was0.103 g, 84.5% on the basis of H1L2). The results of elementalanalysis (%) are as follows: Anal. Calcd: C44H30Cl2N6O5Zn2(%): C, 57.17; H, 3.27; and N, 9.09. Found: C, 57.21; H, 3.72;and N, 9.22. FT-IR (KBr pellet, cm- 1): 3 380 s, 2 924 w, 1571 s, 1 560 s, 1 412 m, 1 301 s, 1 088 m, 831 w, and 718 m. |