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CAS No. : | 6156-78-1 | MDL No. : | MFCD00062552 |
Formula : | C4H14MnO8 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | CESXSDZNZGSWSP-UHFFFAOYSA-L |
M.W : | 245.09 | Pubchem ID : | 93021 |
Synonyms : |
|
Num. heavy atoms : | 13 |
Num. arom. heavy atoms : | 0 |
Fraction Csp3 : | 0.5 |
Num. rotatable bonds : | 0 |
Num. H-bond acceptors : | 8.0 |
Num. H-bond donors : | 4.0 |
Molar Refractivity : | 35.31 |
TPSA : | 117.18 Ų |
GI absorption : | Low |
BBB permeant : | No |
P-gp substrate : | No |
CYP1A2 inhibitor : | No |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -9.44 cm/s |
Log Po/w (iLOGP) : | 0.0 |
Log Po/w (XLOGP3) : | -2.32 |
Log Po/w (WLOGP) : | -2.74 |
Log Po/w (MLOGP) : | -3.77 |
Log Po/w (SILICOS-IT) : | -0.48 |
Consensus Log Po/w : | -1.86 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 2.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | 0.1 |
Solubility : | 310.0 mg/ml ; 1.26 mol/l |
Class : | Highly soluble |
Log S (Ali) : | 0.4 |
Solubility : | 609.0 mg/ml ; 2.49 mol/l |
Class : | Highly soluble |
Log S (SILICOS-IT) : | 0.53 |
Solubility : | 838.0 mg/ml ; 3.42 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 0.0 alert |
Leadlikeness : | 1.0 |
Synthetic accessibility : | 1.0 |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338-P310 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
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 |
---|---|---|
93% | Stage #1: at 90℃; Stage #2: for 1 h; Reflux |
To a 2 L round-bottomed flask, Mn(OAc)2•4H2O (66 g, 0.27 mol) and glacial AcOH (660 mL) were added and the mixture was heated at 90°C to dissolve the components (normally for 10-30 min). The mixture must not be heated under reflux. After cooling, acetic anhydride (96 mL) was added to the mixture with stirring. Three portions of ground potassium permanganate, KMnO4, (11 g, 0.07 mol) were then slowly added with stirring. The mixture was heated under reflux for 1 h (Caution: the added KMnO4 must be dissolved in the reaction mixture. Otherwise the reaction mixture could be bumpy while cooling on the bench Very dangerous). After cooling, water (110 mL) was added and the mixture was kept at room temperature under dark conditions until the dark color of the supernatant solution turned transparent normally within for 2 weeks. The crystalline manganese(III) acetate formed was filtered, washed three times with glacial AcOH, washed twice with dried Et2O, and dried in a desiccator under reduced pressure using KOH as a drying agent, resulting in the bright-brown color of Mn(OAc)3•2H2O (67 g, 93percent yield). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | at 20℃; for 24h;pH 5; | A mixture of Mn(CH3CO2)2·4H2O (0.30 mmol) with H2L (0.30 mmol) and phen (0.30 mmol) in 10 mL distilled water was stirred for half an hour and then stood at room temperature. Pale yellow brick-shaped crystals of 1 were obtained after one day, in approximately 56% yield based on Mn, and the final pH value of the solution was ?5. Anal. Calc. for C21H23N2O7P1Mn1 (Mr = 501.32): C, 50.31; H, 4.62; N, 5.59. Found: C, 50.25; H, 4.73; N, 5.53%. IR data (KBr, cm-1): 3394(s), 3051(m), 2922(m), 2856(m), 1558(s), 1512(m), 1427(s), 1398(m), 1311(m), 1205(m), 1178(s), 1136(s), 1078(m), 1048(m), 1027(m), 931(m), 852(m), 756(m), 735(m), 638(m), 555(m), 513(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | With urea; at 110℃; for 72h;pH 6;Autoclave; | A mixture of Mn(CH3CO2)2·4H2O (0.30 mmol), H2L (0.30 mmol), phen (0.30 mmol) and urea (0.30 mmol) in 12 mL of distilled water was sealed in a Parr Teflon-lined autoclave (23 mL) and heated at 110 C for 3 days. The final pH value was ?6 and yellow column-shaped crystals of 2 were collected in ca. 70% yield based on Mn. Anal. Calc. for C21H19N2O5P1Mn1 (Mr = 465.29): C, 54.21; H, 4.12; N, 6.02. Found: C, 54.12; H, 4.21; N, 5.96%. IR data (KBr, cm-1): 3073(s), 2921(m), 1564(s), 1514(m), 1425(s), 1306(m), 1198(m), 1157(s), 1128(m), 1043(s), 1028(m), 937(m), 856(m), 798(m), 735(m), 638(m), 543(m), 521(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water; at 70℃; for 12h;Reflux; | General procedure: Sn1-xMnxO2 (x = 0.05. 0.10 and 0.15) nanoparticles were synthesized by modified solvothermal method using oxalate as the precursor. The aqueous solutions of metal salts (0.1 M) were prepared in double distilled water. Stoichiometric quantities of tin chloride dihydrate (Merck, 97%) and manganese acetate tetrahydrate (CDH, 99%) were well mixed in 500 mL round bottom flask with constant stirring. 75 mL of di<strong>[1113-38-8]ammonium oxalate</strong> monohydrate (Merck, 99%) was added into the mixture slowly with constant stirring to minimize the agglomeration and to promote faster precipitation. A pale yellow suspension was immediately formed. Approximately 75 mL of ethanol (Merck) was also added to the reaction mixture in order to reduce its boiling temperature and the mixture was refluxed for 12 h at 70 C in a closed environment so that the volume of reaction mixture remains constant. The precipitate was separated from the solution by centrifugation and washed with double distilled water to remove water soluble impurities and finally with acetone. The precipitates were dried in oven at 55 C for 1 h. Pale yellow powders of Mn doped tin oxalate precursors were obtained. On the basis of thermogravimetric analysis, grey powders of Sn1xMnxO2 (x = 0.05, 0.10 and 0.15) nanoparticles were obtained by the decomposition of precursors at 600 C for 6 h in nitrogen atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water; at 70℃; for 12h;Reflux; | General procedure: Sn1-xMnxO2 (x = 0.05. 0.10 and 0.15) nanoparticles were synthesized by modified solvothermal method using oxalate as the precursor. The aqueous solutions of metal salts (0.1 M) were prepared in double distilled water. Stoichiometric quantities of tin chloride dihydrate (Merck, 97%) and manganese acetate tetrahydrate (CDH, 99%) were well mixed in 500 mL round bottom flask with constant stirring. 75 mL of di<strong>[1113-38-8]ammonium oxalate</strong> monohydrate (Merck, 99%) was added into the mixture slowly with constant stirring to minimize the agglomeration and to promote faster precipitation. A pale yellow suspension was immediately formed. Approximately 75 mL of ethanol (Merck) was also added to the reaction mixture in order to reduce its boiling temperature and the mixture was refluxed for 12 h at 70 C in a closed environment so that the volume of reaction mixture remains constant. The precipitate was separated from the solution by centrifugation and washed with double distilled water to remove water soluble impurities and finally with acetone. The precipitates were dried in oven at 55 C for 1 h. Pale yellow powders of Mn doped tin oxalate precursors were obtained. On the basis of thermogravimetric analysis, grey powders of Sn1xMnxO2 (x = 0.05, 0.10 and 0.15) nanoparticles were obtained by the decomposition of precursors at 600 C for 6 h in nitrogen atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water; at 70℃; for 12h;Reflux; | General procedure: Sn1-xMnxO2 (x = 0.05. 0.10 and 0.15) nanoparticles were synthesized by modified solvothermal method using oxalate as the precursor. The aqueous solutions of metal salts (0.1 M) were prepared in double distilled water. Stoichiometric quantities of tin chloride dihydrate (Merck, 97%) and manganese acetate tetrahydrate (CDH, 99%) were well mixed in 500 mL round bottom flask with constant stirring. 75 mL of di<strong>[1113-38-8]ammonium oxalate</strong> monohydrate (Merck, 99%) was added into the mixture slowly with constant stirring to minimize the agglomeration and to promote faster precipitation. A pale yellow suspension was immediately formed. Approximately 75 mL of ethanol (Merck) was also added to the reaction mixture in order to reduce its boiling temperature and the mixture was refluxed for 12 h at 70 C in a closed environment so that the volume of reaction mixture remains constant. The precipitate was separated from the solution by centrifugation and washed with double distilled water to remove water soluble impurities and finally with acetone. The precipitates were dried in oven at 55 C for 1 h. Pale yellow powders of Mn doped tin oxalate precursors were obtained. On the basis of thermogravimetric analysis, grey powders of Sn1xMnxO2 (x = 0.05, 0.10 and 0.15) nanoparticles were obtained by the decomposition of precursors at 600 C for 6 h in nitrogen atmosphere. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | for 0.5h; | General procedure: A mixture of equal molar 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol), Mn(OAc)24H2O (73.5 mg, 0.3 mmol) was dissolved in the MF/H2O mixed solvents (v/v, 1:1, 12 mL) with stirring for ca. 30 min. The resulting solution was filtered and left to stand at room temperature. Colorless block crystals of 1 suitable for X-ray single-crystal diffraction were obtained by slow evaporation of the solvents after three weeks in about 70% yield based on 1,2-H2BDC-Cl4. Anal. Calc. for C12H14Cl4MnN2O8 (1): C, 28.21; H, 2.76 ;N, 5.48. Found: C, 28.37; H, 2.79; N, 5.36%. IR (cm1): 3266 br, 3091 m, 2946 m, 2926 m, 1656 s, 1602 vs 1529 s, 1426 s, 1396 s, 1372 s, 1342 s, 1269 m, 1205 m, 1156 w, 1128 w, 932 w, 913 m,831 w, 780 m, 655 s, 616 m, 572 m. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
30% | for 0.5h; | The same synthetic procedure as that for 1 was used except that MF was replaced by DMF, affording colorless block crystals of 2 in about 30% yield based on 1,2-H2BDC-Cl4. Anal. Calc. for C11H11Cl4-MnNO7 (2): C, 28.35; H, 2.38; N, 3.01. Found: C, 28.12; H, 2.36; N, 3.25%. IR (cm1): 3311 br, 2958 m, 2930 m, 1671 s, 1604 s, 1526 m, 1426 s, 1384 s, 1342 s, 1253 m, 1202 w, 1125 m, 1095m, 1060 w, 925 w, 913 m, 828 m, 652 s, 612 m, 541 m. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | for 0.5h; | The procedure was the same as that for 1 except that the solvent MF was replaced by DEF, affording colorless block crystals of 3 in about 40% yield based on 1,2-H2BDC-Cl4. Elemental analysis calcd for C26H38Cl8Mn2N2O18: C, 29.46; H, 3.61; N, 2.64. Found: C, 30.12; H, 3.59; N, 2.68%. IR (KBr, cm1): 3419 br, 3078 s, 2933 s, 1657 vs 1614 s, 1566 s, 1449 s, 1371 vs 1312 m, 1251 m, 1110m, 1061 w, 968 m, 807 m, 781 s, 728 s, 680 m. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Ca. 70% | In water; for 0.5h; | General procedure: A mixture of equal molar 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol), Mn(OAc)24H2O (73.5 mg, 0.3 mmol) was dissolved in the MF/H2O mixed solvents (v/v, 1:1, 12 mL) with stirring for ca. 30 min. The resulting solution was filtered and left to stand at room temperature. Colorless block crystals of 1 suitable for X-ray single-crystal diffraction were obtained by slow evaporation of the solvents after three weeks in about 70% yield based on 1,2-H2BDC-Cl4. Anal. Calc. for C12H14Cl4MnN2O8 (1): C, 28.21; H, 2.76;N, 5.48. Found: C, 28.37; H, 2.79; N, 5.36%. IR (cm1): 3266 br,3091 m, 2946 m, 2926 m, 1656 s, 1602 vs 1529 s, 1426 s, 1396 s,1372 s, 1342 s, 1269 m, 1205 m, 1156 w, 1128 w, 932 w, 913 m,831 w, 780 m, 655 s, 616 m, 572 m. |
70% | In water; for 0.5h; | A mixture of equal molar 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol),Mn(OAc)24H2O (73.5 mg, 0.3 mmol) was dissolved in the MF/H2O mixed solvents (v/v, 1:1, 12 mL) with stirring for ca. 30 min.The resulting solution was filtered and left to stand at roomtemperature. Colorless block crystals of 1 suitable for X-ray single-crystal diffraction were obtained by slow evaporation of thesolvents after three weeks in about 70% yield based on 1,2-H2BDC-Cl4. Anal. Calc. for C12H14Cl4MnN2O8 (1): C, 28.21; H, 2.76;N, 5.48. Found: C, 28.37; H, 2.79; N, 5.36%. IR (cm1): 3266 br,3091 m, 2946 m, 2926 m, 1656 s, 1602 vs 1529 s, 1426 s, 1396 s,1372 s, 1342 s, 1269 m, 1205 m, 1156 w, 1128 w, 932 w, 913 m,831 w, 780 m, 655 s, 616 m, 572 m. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Ca. 40% | In water; for 0.5h; | General procedure: A mixture of equal molar 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol), Mn(OAc)24H2O (73.5 mg, 0.3 mmol) was dissolved in the MF/H2O mixed solvents (v/v, 1:1, 12 mL) with stirring for ca. 30 min. The resulting solution was filtered and left to stand at room temperature. Colorless block crystals of 1 suitable for X-ray single-crystal diffraction were obtained by slow evaporation of the solvents after three weeks in about 70% yield based on 1,2-H2BDC-Cl4. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Ca. 30% | In water; for 0.5h; | General procedure: A mixture of equal molar 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol), Mn(OAc)24H2O (73.5 mg, 0.3 mmol) was dissolved in the MF/H2O mixed solvents (v/v, 1:1, 12 mL) with stirring for ca. 30 min. The resulting solution was filtered and left to stand at room temperature. Colorless block crystals of 1 suitable for X-ray single-crystal diffraction were obtained by slow evaporation of the solvents after three weeks in about 70% yield based on 1,2-H2BDC-Cl4. |
30% | In water; for 0.5h; | General procedure: A mixture of equal molar 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol),Mn(OAc)24H2O (73.5 mg, 0.3 mmol) was dissolved in the MF/H2O mixed solvents (v/v, 1:1, 12 mL) with stirring for ca. 30 min.The resulting solution was filtered and left to stand at roomtemperature. Colorless block crystals of 1 suitable for X-ray single-crystal diffraction were obtained by slow evaporation of thesolvents after three weeks in about 70% yield based on 1,2-H2BDC-Cl4 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
55% | With sodium hydroxide; In ethanol; at 130℃; for 144h;pH 7;High pressure; | Compound 1 was obtained by reaction of Mn(OAc)2·4H2O (0.025 g, 0.1 mmol), H2dtb (0.039 g, 0.1mmol), bpe (0.018 g, 0.1mmol), ethanol (2.0 mL), and distilled water (15.0 mL) under hydrothermal conditions. The pH of the reaction solution was adjusted to 7 with 1M NaOH; it was heated to 130 C for 6 days and then cooled to room temperature at 5 C/h. Colorless crystals of 1 (0.021 g, 55% yield) were collected. Anal. Calcd. forC26H22MnN4O11S2: C, 45.55; H, 3.23; N, 8.17. Found: C, 46.04; H, 3.61; N, 8.36%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With sodium hydroxide; In ethanol; at 130℃; for 144h;pH 7;High pressure; | Compound 2 was synthesized analogously to 1 except that bpe was replaced by bpa. Colorless block X-ray-quality crystals (0.026 g, 60% yield) were obtained. Anal. Calcd for C26H24MnN4O11S2: C, 45.42; H, 3.51; N, 8.15. Found: C, 45.54; H, 3.74; N, 8.71. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
56% | With sodium hydroxide; In ethanol; water; at 130℃; for 144h;pH 7;High pressure; | Compound 3 was synthesized analogously to 1 except that bpe was replaced by phen. Colorless block X-ray-quality crystals (0.022 g, 56% yield) were obtained. Anal. Calcd for C26H14MnN4O8S2: C, 49.61; H, 2.24; N, 8.90. Found: C, 49.04; H, 2.74; N, 8.71. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | General procedure: A solution containing pyridoxal (neutral) (0.406 g, 2.0 mmol)and Zn(OAc)2*2H2O (0.220 g, 1.0 mmol) in methanol (15 ml) was cooled at 0 C. To this solution, triethylenetetramine (0.149 ml, 1.0 mmol) in methanol (10 ml) was added drop wise over a period of 10 min. After stirring at 0 C for 15 min, a solution of 2 N sodium hydroxide (1.0 ml, 2.0 mmol) was added and the reaction mixture was stirred at room temperature for 1 h. Pale yellow crystals of ZnL*2H2O (1), suitable for X-ray structure determination, were obtained by slow evaporation of methanol from the reaction mixture, at room temperature. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | In water; for 0.5h; | General procedure: A mixture of equal molar 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol),Mn(OAc)24H2O (73.5 mg, 0.3 mmol) was dissolved in the MF/H2O mixed solvents (v/v, 1:1, 12 mL) with stirring for ca. 30 min.The resulting solution was filtered and left to stand at roomtemperature. Colorless block crystals of 1 suitable for X-ray single-crystal diffraction were obtained by slow evaporation of thesolvents after three weeks in about 70% yield based on 1,2-H2BDC-Cl4 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | In ethanol; water; for 0.5h; | An ethanol solution (2 mL) of 1,2-H2BDC-Cl4 (91.2 mg, 0.3 mmol) was added to an aqueous (6 mL) solution of Mn(OAc)2·4H2O (73.5 mg, 0.3 mmol). Then, the mixture was stirred for ca. 30 min. The resulting solution was filtered and left to stand at room temperature. Yellow block-shaped crystals suitable for X-ray analysis were obtained after two weeks in 65 % yield (87.1 mg, on the basis of 1,2-H2BDCCl4). - Anal. for C16H20Cl8Mn2O18 (%): calcd. C 21.50, H 2.26; found C 21.26, H 2.27. - IR (KBr pellet): nu = 3423 (br), 1646 (s), 1590 (vs), 1530 (m), 1433 (s), 1404 (m), 1344 (s), 1212 (w), 1131 (w), 918 (w), 843 (m), 672 (m), 650 (m), 615 (m) cm-1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | In ethanol; water; for 0.5h; | The same synthetic procedure as that described for 1 was used except that KNO3 (60.6 mg, 0.6 mmol) was added, affording yellow block-shaped crystals of 2 upon slow evaporation of the solvent in 40 % yield ( 48.5 mg, on the basis of 1,2-H2BDC-Cl4). - Anal. for C16H8Cl8K2MnO12 (%):calcd. C 23.76, H 1.00; found C 24.03, H 1.02. - IR (KBr pellet): nu = 3407 (br), 1592 (vs), 1532 (m), 1426 (s), 1388 (m), 1339 (s), 1207 (w), 1127 (w), 938 (w), 904 (w), 663 (m), 647 (m), 618 (m) cm-1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water; for 24h;Inert atmosphere; | 0.1 mol (29.08 g) of Ni(NO3)2*6H2O, 0.1 mol (29.70 g) of Co(NO3)2*6H2O, and 0.1 mol (24.76 g) of Mn(CH3COO)2*4H2O were dissolved in 150 mL H2O, and stirred at 200 rpm. 0.3 mol (43.06 g) of (NH4)2C2O4*H2O were added to the precursor mixture solution with argon atmosphere for 24 h. The obtained Ni1/3Co1/3Mn1/3C2O4*xH2O were washed by using methanol (CH3OH) and chloroform (CHCl3) and dried at 100 C for 2 h for TGA. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
24% | General procedure: Erbium(III) nitrate pentahydrate (0.125mmol), the sodium carboxylate salt (4 mmol; 1: trimethylacetate hydrate based on an assumption of three waters of hydration; 2: sodium benzoate; 3: sodium salicylate), and <strong>[89-73-6]salicylhydroxamic acid</strong> (2mmol) were mixed in 10 mL of DMF resulting in a cloudy, white mixture for 1 and 2 or a clear, colorless solution for 3. In a separate beaker, manganese(II) acetate tetrahydrate (2 mmol) was dissolved in 10mL of DMF resulting in an orange/red solution. The two solutions were mixed resulting in a dark brown solution and then allowed to stir overnight. The solution was then filtered to remove a dark brown precipitate, which was discarded. The filtrate was then prepared for crystal growth (details below). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
27% | General procedure: Erbium(III) nitrate pentahydrate (0.125mmol), the sodium carboxylate salt (4 mmol; 1: trimethylacetate hydrate based on an assumption of three waters of hydration; 2: sodium benzoate; 3: sodium salicylate), and <strong>[89-73-6]salicylhydroxamic acid</strong> (2mmol) were mixed in 10 mL of DMF resulting in a cloudy, white mixture for 1 and 2 or a clear, colorless solution for 3. In a separate beaker, manganese(II) acetate tetrahydrate (2 mmol) was dissolved in 10mL of DMF resulting in an orange/red solution. The two solutions were mixed resulting in a dark brown solution and then allowed to stir overnight. The solution was then filtered to remove a dark brown precipitate, which was discarded. The filtrate was then prepared for crystal growth (details below). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
17% | General procedure: Erbium(III) nitrate pentahydrate (0.125mmol), the sodium carboxylate salt (4 mmol; 1: trimethylacetate hydrate based on an assumption of three waters of hydration; 2: sodium benzoate; 3: sodium salicylate), and <strong>[89-73-6]salicylhydroxamic acid</strong> (2mmol) were mixed in 10 mL of DMF resulting in a cloudy, white mixture for 1 and 2 or a clear, colorless solution for 3. In a separate beaker, manganese(II) acetate tetrahydrate (2 mmol) was dissolved in 10mL of DMF resulting in an orange/red solution. The two solutions were mixed resulting in a dark brown solution and then allowed to stir overnight. The solution was then filtered to remove a dark brown precipitate, which was discarded. The filtrate was then prepared for crystal growth (details below). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
44% | 2, 5-di(2?,4?-dicarboxylphenyl) pyridine (0.041 g, 0.1 mmol) and(NH4)2C2O4·H2O (0.016 g, 0.1 mmol) in a solution of water/DMF (v/v = 4.0,12 mL) were mixed with an aqueous solution (10 mL) of Mn(CH3COO)2·4H2O (0.0295 g, 0.12 mmol). After stirring for 20 min in air, the pH value was adjusted to5.5 with nitric acid, and the mixture was placed into 25 mL Teflon-lined autoclaveunder autogenous pressure being heated at 145 C for 72 h, then the autoclavewas cooled over a period of 24 h at a rate 5 C/h. After filtration, the product waswashed with distilled water and then dried, colorless crystals of title polymerwere obtained suitable for X-ray diffraction analysis. Yield: 0.011 g (44% based onMn element)). Elemental analysis (%): calcd for C44H36Mn4N2O28: C 41.93, H 2.88,N 2.22, O 35.54, Mn 17.43, found: C 40.86, H 2.49, N 2.14, O 35.39, Mn 17.36. IR(KBr pellet, cm-1): 3486 (br), 1708(s), 1643(s), 1603(s), 1410(m), 1387(s),1139(m), 817(s), 784(m), 668(s), IR spectra see Fig. S1 for details. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 120℃; for 96h;High pressure; Autoclave; | A mixture of H2Nbdc(0.1 mmol, 21.2 mg), Bipyp (0.2 mmol, 19.6 mg),Mn(Ac)2 · 4H2O (0.1 mmol, 24.9 mg), and H2O(6.0 mL) was sealed in a 23 mL Teflon-lined autoclave,heated to 120C for 4 days, then cooled at 5 K/hto room temperature. Colourless block crystals wereobtained.For C29H28N4O16Mn2anal. calcd, %: C, 43.63; H, 3.53; N, 7.02.Found, %: C, 43.42; H, 3.68; N, 7.19. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium hydroxide; at 120℃; for 96h;High pressure; Autoclave; | A mixture of H2Nbdc(0.1 mmol, 21.1 mg), Bipye (0.2 mmol, 18.5 mg),Mn(Ac)2 · 4H2O (0.1 mmol, 24.5 mg), H2O (6.0 mL),and KOH (0.1 mmol) were sealed in a 23 mL Teflonlinedautoclave, heated to 120C for 4 days, thencooled at 5 Kappa/h to room temperature. For C28H26N4O16Mn2anal. calcd, %: C, 42.87; H, 3.34; N, 7.14.Found, %: C, 42.70; H, 3.42; N, 7.29. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
46.7% | at 140℃; for 72h;Autoclave; High pressure; | General procedure: A mixture containing Mn(OAc)2·4H2O (24.5mg, 0.1mmol), L1 (36.6mg, 0.1mmol) and H2DCTP (23.5mg, 0.1mmol) was dissolved in 10mL of distilled water at room temperature. The suspension was put into a 25mL Teflon-lined autoclave and kept under autogenous pressure at 140C for 3days. After slow cooling to room temperature and overnight drying, yellow block crystals were filtered and washed with distilled water, Yield: 51.8% referred to Mn(OAc)2·4H2O. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51.8% | at 140℃; for 72h;Autoclave; High pressure; | A mixture containing Mn(OAc)2·4H2O (24.5mg, 0.1mmol), L1 (36.6mg, 0.1mmol) and H2DCTP (23.5mg, 0.1mmol) was dissolved in 10mL of distilled water at room temperature. The suspension was put into a 25mL Teflon-lined autoclave and kept under autogenous pressure at 140C for 3days. After slow cooling to room temperature and overnight drying, yellow block crystals were filtered and washed with distilled water, Yield: 51.8% referred to Mn(OAc)2·4H2O. Anal. Calc. for C56H50Cl2MnN8O6 (Mr=1056.88): C, 63.64; H, 4.77; N, 10.60; Found: C, 63.86; H, 4.92; N, 10.38%. IR (solid KBr pellet, cm-1): 3445(s), 3042(w), 2917(w), 1577(s), 1509(m), 1406(s), 1368(s), 1230(m), 1077(m), 902(w), 796(m), 750(s), 655(m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
53.8% | In water; at 140℃; for 72h;Autoclave; High pressure; | General procedure: A mixture containing Mn(OAc)2·4H2O (24.5mg, 0.1mmol), L1 (36.6mg, 0.1mmol) and H2DCTP (23.5mg, 0.1mmol) was dissolved in 10mL of distilled water at room temperature. The suspension was put into a 25mL Teflon-lined autoclave and kept under autogenous pressure at 140C for 3days. After slow cooling to room temperature and overnight drying, yellow block crystals were filtered and washed with distilled water, Yield: 51.8% referred to Mn(OAc)2·4H2O. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
37% | at 85℃; for 48h;Autoclave; High pressure; | A mixture of Mn(OAc)24H2O (0.2 mmol, 0.0490 g) and 1,4-H2NDC (0.2 mmol, 0.0432 g) was dissolved in the mixed solventsof CH3OH/CH3CH2OH/DMF/H2O (6/1/2/2, 11 mL) and then transferredto and sealed in a 25mL Teflon lined stainless steel container,which was heated at 85 C for 2 days. After being cooled to roomtemperature at a rate of 3 C h1, pale red crystals of 1 werecollected by filtration and washed with water and ethanol. Yield of37% (based on Mn). Anal. calcd for C30H31Mn2NO12 (%): C, 50.95; H,4.38; N, 1.98. Found: C, 50.89; H, 4.35; N, 1.95. IR (KBr pellet, cm1):3433(m), 2972(w), 1660(m), 1573(s), 1457(w), 1417(s), 1365(s),1263(w), 1045(w), 830(w), 786(w), 573(w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
39% | In methanol; at 85℃; for 48h;Autoclave; High pressure; | General procedure: A mixture of Mn(OAc)24H2O (0.2 mmol, 0.0490 g) and 1,4-H2NDC (0.2 mmol, 0.0432 g) was dissolved in the mixed solventsof CH3OH/CH3CH2OH/DMF/H2O (6/1/2/2, 11 mL) and then transferredto and sealed in a 25mL Teflon lined stainless steel container,which was heated at 85 C for 2 days. After being cooled to roomtemperature at a rate of 3 C h1, pale red crystals of 1 werecollected by filtration and washed with water and ethanol. Yield of37% (based on Mn). Anal. calcd for C30H31Mn2NO12 (%): C, 50.95; H,4.38; N, 1.98. Found: C, 50.89; H, 4.35; N, 1.95. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With ascorbic acid; In water; at 60℃; for 5h;pH 5;Inert atmosphere; | weight 180.91g ferrous acetate, 363.22g manganese tetrahydrate acetate, ascorbic acid 1.5g, dissolved in appropriate amount of water that is preparation of iron and manganese mixed solution A; 14.63g copper nitrate, dissolved in small amount of water, this is solution B. Into the reaction flask added the 402 g of <strong>[1113-38-8]ammonium oxalate</strong> and appropriate amount of water, Ammonium oxalate concentration is 1.0mol / L, into the reaction flask pass nitrogen, flow meter set at 600 ml / min, system pH is 5, the reactor temperature is controlled at 60 C and heated to <strong>[1113-38-8]ammonium oxalate</strong> completely dissolved. In the agitation state, simultaneous added the iron and manganese mixed solution A and copper nitrate solution B to the system by using parallel flow method. The drip rate of iron-manganese mixed solution A is 4 L / h, and the drip rate of copper sulfate solution B is 0.5L / h, 1L / h, 2L / h gradually increased, after the drop, in the state of stirring to continue aging 5h, stirring speed is 100r / min, the intermediate is washed with methanol, respectively, dry at 75 C, where dry time will be 3 hours, the chemical composition is Fe0.4Mn.57Cu0.03C2O4 . 2H2OCopper gradient doped intermediates, that is D50 is 100muM, see SEM fig1 in D. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Reaction of K6[(OH)TeNb5O18]15H2O with Mn(OAc)24H2O inthe presence of H2O2 was done in the same way using 2.0 g ofthe telluropentaniobate, but instead of a crystalline product (nocrystallization occurred upon cooling), evaporation of the solutionin air gives only amorphous brown precipitate. In attempts todecrease the solubility by introduction of Na+, as is in the case ofthe polyoxonibates, addition of a several drops of 1 M Na2SO4 tothe reaction solution resulted in the formation of a tractable brownprecipitate. IR (KBr, cm1): 3400 (s), 1632 (m), 871 (s), 772 (s), 687(s), 528(s), 436 (s); TGA: weight loss 8.5% (at 150 C), which is inaccord with the calculated value of 8.9%. EDS found K, Na, Nb, Te,Mn (%): 14.8, 1.2, 38.4, 10.2, 2.4; calc. for K9NaNb10Te2O38Mn(H2O)12 K, Na, Nb, Te, Mn (%):14.4, 1.0, 38.1, 10.5, 2.3. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | General procedure: 2.00 g (1.5 mmol) of K7H[Nb6O19]13H2O was dissolved in 20mL of distilled water under gentle heating (60 C) and stirring, afterthat 0.27 g (0.7 mmol) of Na2EDTA and 0.08 g (1 mmol) of KOHwere added to the solution. Separately, 0.18 g (0.7 mmol) of Mn(OAc)24H2O was dissolved in 2.0 mL of hot water and added dropwiseto the hexaniobate solution. Then, a few drops of 30% H2O2were added to the reaction mixture resulting in brown colorationof the solution. Some brown precipitate was filtered off, and finalsolution was allowed to cool to r.t. and kept in a fridge at 2 Cfor 24 h for crystallization. Orange polyhedral crystals were collectedby filtration, washed with ethanol, diethyl ether, and driedin air. Yield 40%. Purity of the product was confirmed with XRPD(Fig. S1). IR (KBr, cm1): 3291 (s), 1637 (m), 861(s), 775 (s), 689(s), 527 (s), 435 (s). TGA: weight loss 15% (at 150 C), which is inaccord to calculated 15.6% for 18.5 water molecules of crystallization.ICP-AES found K, Na, Mn, Nb (%): 14.0, 1.6, 2.0, 44.0. Calcd for1 found K, Na, Mn, Nb (%): 14.4, 1.8, 2.2, 44.4. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With ammonia; at 120℃; for 24h; | In a 7ml Teflon reaction vessel 0.5 mmole Orotic Acid, 0.5 mmole Mn(Ac)2.4H2O and 5 ml 25% ammonia solution was taken. The reaction vessel was then placed in a stainless steel reactor and heated at 120C in a high precision programmed oven at the heating rate of 20C /hour for a period of 24 hours. After heating the reaction vessel was cooled at the same rate as it was heated.The light brown clear solution thus obtained was filter and kept for crystallization at room temperature. After three days air stable light green and black block shaped crystals suitable for X-ray diffraction was collected from same reaction mixture.The color of complex 2 can vary in between dark green or black. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With ammonium dimolybdate; ammonium chloride; In neat (no solvent, solid phase); at 140 - 220℃; for 6.5h; | General procedure: The synthetic steps of MPc (COOH) 4Cl8 (Scheme 1). A mixture of1.0025 g of <strong>[81742-10-1]3,6-dichloro-1,2,4-benzenetricarboxylic anhydride</strong>,6.0000 g of urea, 0.3654 g of Mn(CH3COOH)2·4H2O, 0.25 g of NH4Cland 0.1200 g of (NH4)2Mo2O7 in 100 mL three-necked flask was heatedat 140 C for 0.5 h with magnetic stirrer and reflux condenser, and thenkept at 220 C for 6 h under ambient air conditions. The by-productswere washed with water followed by 6 mol L-1 hydrochloric acid forseveral times. Then the purification of blue solid was achieved by refluxingwith 150 mL of acetone and trichloromethane about 12 h.The obtained octachloro-tetracarboxamide phthalocyanine was hydrolyzedwith 100 mL of 2.0 mol·L-1 sodium hydroxide solution at 100 C for 12 h, filtered, and the filtrate was adjusted to pH=1 withhydrochloric acid, a large amount of precipitates were produced andfiltered by the G4 sand core funnel, the filter cake was washed first withdeionized water until the filtrate was neutral. Then the filter cake waswashed with in proper order. The solid product was vacuum dried at100 C. The as-prepared MPcTcCl8 were washed by chloroform,ethanol, ether, acetone and THF respectively, dried in vacuum overnightat 100 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
38.4% | In water; at 140℃; for 82h;High pressure; Autoclave; | A mixture of L (34.6 mg, 0.1 mmol), Mn(OAc)2*4H2O (49.2 mg, 0.2 mmol), 1,4-H2NDC (43.2 mg, 0.2 mmol), and H2O (10.0 mL) was sealed in a 25.0 mL Teflon-lined stainless steel vessel, which was then heated to 140 C within 10 h and kept at 140 C for 72 h followed by slowly cooled to 25 C within 24 h. Colorless blocked crystals of NCST-3 were collected for single crystal X-ray diffraction analysis. Yield: 38.4% based on L. Anal. Calc. for C34H34MnN4O5 (Fw 633.59): C, 64.45; H, 5.41; N, 8.84%. Found: C, 64.58; H, 5.67; N, 8.61%. IR (KBr, cm1): 3427s, 3111w, 2942w, 1573s, 1508 m, 1406s,1363s, 1209w, 1078 m, 802 m. |
Tags: 6156-78-1 synthesis path| 6156-78-1 SDS| 6156-78-1 COA| 6156-78-1 purity| 6156-78-1 application| 6156-78-1 NMR| 6156-78-1 COA| 6156-78-1 structure
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