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CAS No. : | 586372-53-4 | MDL No. : | MFCD34165581 |
Formula : | C9H15O9P3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | QNXIXVZKHKBGHY-UHFFFAOYSA-N |
M.W : | 360.13 | Pubchem ID : | 13669035 |
Synonyms : |
|
Signal Word: | Danger | Class: | 8 |
Precautionary Statements: | P501-P260-P234-P264-P280-P390-P303+P361+P353-P301+P330+P331-P363-P304+P340+P310-P305+P351+P338+P310-P406-P405 | UN#: | 3261 |
Hazard Statements: | H314-H290 | Packing Group: | Ⅲ |
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 |
---|---|---|
92% | With hydrogenchloride; water for 24h; Heating; | |
92% | In hydrogenchloride for 24h; Heating; | |
92% | With hydrogenchloride In water for 20h; Reflux; |
80.3 % | With hydrogenchloride In water at 110℃; | 1.S3-3.S3 S3: Synthesis of 1,3,5-benzenetrimethylphosphonic acid At room temperature, the intermediate II (7.0 g, 13.25 mmol) prepared in the previous step and 130 mL of concentrated hydrochloric acid were successively added to a 250 mL reaction flask, and the reaction was refluxed at 110° C. for 20 h, monitored by TLC [V (dichloromethane): V (methanol )=8:1] After the reaction was completed, cooling and decompression removed excess water and HCl to obtain 4.68g white solid, which was recrystallized with methanol/water (volume ratio 7:1) mixed solution to obtain a large amount of white crystal block III, which was vacuum-dried (dried at 50-55°C for 8-10h) to obtain 3.83g of white crystals with a yield of 80.3%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
280 mg | In methanol; water at 18℃; |
Yield | Reaction Conditions | Operation in experiment |
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33% | In ethanol; water addn. of bipyridine to soln. of phosphonic acid deriv. in aq. ethanol, mixing with aq. soln. of copper compd., heating at 95-100°C for 3 d; isolation of crystals, X-ray anal.; |
Yield | Reaction Conditions | Operation in experiment |
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at 20℃; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
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at 60℃; for 0.0833333h; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
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at 60℃; for 0.0833333h; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
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86% | at 140℃; for 96h; Autoclave; | H6L1 (0.25 mmol, 0.090 g), Pb(ac)2·3H2O (0.375 mmol, 0.1422 g), and 10 mL of water were mixed and stirred in a Teflon-lined autoclave. Afterward, it was sealed and heated at 140 °C for 4 days and allowed to cool to room temperature in a time period of 24 hours. Colorless plate crystals of 1 (0.1455 g) were collected and washed with deionized water in satisfying yield (86 %, based on metal). Elemental analysis (%) calcd for C18H26O19P6Pb3 (1353.78): C 15.97, H 1.94; found: C 15.90, H 2.03. IR(KBr, cm-1): 3423 (b, m), 2895 (w), 1637 (w), 1599 (m), 1454 (w), 1416 (w), 1227 (m), 1125 (s), 1049 (vs), 938 (s), 909 (m), 875 (m), 741 (m), 706 (m), 631 (w), 509 (m), 488 (w) (see Figure S6). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
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at 180℃; for 72h; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
26.44% | In water at 160℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen fluoride at 80℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen fluoride; tetrapropylammonium hydroxide at 80℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
82% | With hydrogen fluoride at 80℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
41% | With sodium hydroxide In water at 140℃; for 72h; Autoclave; High pressure; | 2.6. Synthesis of complex [CuH4L2(2, 2′-bipy)]n (4) The preparation of 4 was similar to that of 3 except the displacementof 4, 4′-bipy with 2, 2′-bipy. Blue crystals were obtained andwashed with deionized water. Yield: 27.1 mg (41%, based on Cu). Anal.Calcd. For C19H21N2O9P3Cu: C, 39.492; H, 3.663; N, 4.848%. Found:C, 39.60; H, 3.32; N, 4.52%. Main IR data (KBr, cm-1): 3424 (s), 3116(w), 2912 (w), 1651 (w), 1603 (s), 1495 (w), 1410 (w), 1235 (s), 1171(m), 1137 (w), 1035 (m), 991 (m), 932 (m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
22% | With zinc perchlorate; sodium hydroxide In water at 140℃; for 72h; Autoclave; High pressure; | 2.7. Synthesis of complex [Cu2(H4L2)2(2, 2′-bipy)2(H2O)4] (5) H6L2 (0.05mmol, 0.018g), 2, 2′-bipy (0.155mmol, 0.0242 g),Cu(NO3)2·3H2O (0.048mmol, 0.0117 g), Zn(ClO4)2·6H2O (0.051mmol,0.019g) and 3mL of water were mixed in 10mL vial. Then,50 μL 1 mol/L NaOH was added. The hydrothermal reaction wasconducted under the conditions of 1. Blue crystals were obtained andwashed with deionized water. Yield: 16mg (22%, based on Cu). Anal.Calcd. For C38H50N4O22P6Cu2: C, 37.17; H, 4.11; N, 4.56%. Found: C,37.51; H, 4.41; N, 4.15%. Main IR data (KBr, cm-1): 3443 (m), 3081 (m),1605 (s), 1475 (m), 1445 (s), 1254 (w), 1088 (s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | With sodium hydroxide In water at 140℃; for 72h; Autoclave; High pressure; | 2.5. Synthesis of complex [Cu2H2L2(4, 4′-bipy)(H2O)2]n (3) H6L2 (0.05mmol, 0.0176 g), 4, 4′-bipy (0.158mmol, 0.0246 g),Cu(NO3)2·3H2O (0.1mmol, 0.0240 g) and 3 mL of water were mixed in10 mL vial. Then, 50 μL 1 mol/L NaOH was added. The hydrothermalreaction was performed on the same conditions with 1. Blue crystalswere collected and washed with deionized water. Yield: 29.8 mg (45%,based on Cu). Anal. Calcd. For C19H23N2O11P3Cu2: C, 33.79; H, 3.43;N, 4.15%. Found: C, 33.46; H, 3.72; N, 4.48%. Main IR data (KBr, cm-1): 3386 (s), 3099 (w), 2903 (w), 1611 (s), 1492 (m), 1417 (w), 1222(m), 1148 (w), 1070 (s), 927 (s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
28% | With pyridine-4-carbonitrile; sodium hydroxide In water at 140℃; for 72h; High pressure; | 2.5. Synthesis of complex [Cd4(H2bmt)2(H2O)]n (3) H6bmt (0.05 mmol, 0.018 g), 4-Cyanopyridine (0.151 mmol,0.0157 g), Cd(NO3)2·4H2O (0.105 mmol, 0.0324 g) and 3 mL water were mixed in 10 mL vial. Then, 50 μL 1 mol/L NaOH was added. The hydrothermal reaction was conducted under the same conditions of 1. Colourless crystals were collected and washed with deionized water. Yield: 18.51 mg (28%, based on Cd). Anal. Calcd. For C18H24O19P6Cd4:C, 18.324; H, 2.05%. Found: C, 18.67; H, 2.43%. Main IR data (KBr,cm-1): 3450 (s), 2910 (w), 1602 (s), 1456 (m), 1410 (s), 1384 (w), 1191(w), 1084 (s), 985(s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
64% | With sodium hydroxide In water at 140℃; for 72h; High pressure; | 2.5. Synthesis of complex [Cd4(H2bmt)2(H2O)]n (3) General procedure: H6bmt (0.05 mmol, 0.018 g), 4-Cyanopyridine (0.151 mmol,0.0157 g), Cd(NO3)2·4H2O (0.105 mmol, 0.0324 g) and 3 mL water were mixed in 10 mL vial. Then, 50 μL 1 mol/L NaOH was added. The hydrothermal reaction was conducted under the same conditions of 1. Colourless crystals were collected and washed with deionized water. Yield: 18.51 mg (28%, based on Cd). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | With sodium hydroxide In water at 140℃; for 72h; High pressure; | 2.7. Synthesis of complex [Zn(H4bmt)(2, 2′-bipy)]n (5) H6bmt (0.05mmol, 0.0179 g), 2, 2′-bipy (0.152 mmol, 0.0238 g), Zn(NO3)2·6H2O (0.103mmol, 0.03 g) and 3mL water were mixed in 10mL vial. Then, 50 μL 1 mol/L NaOH was added. The hydrothermal reaction was performed on the same conditions with 1. Colourless crystals were collected and washed with deionized water. Yield: 41.59mg (58%, based on Zn). Anal. Calcd. For C19H21N2O9P3Zn: C, 39.37; H,3.65; N, 4.83%. Found: C, 39.74; H, 3.26; N, 5.12%. Main IR data (KBr,cm-1): 3424 (s), 3078 (w), 2918 (w), 1647 (m), 1603 (s), 1475 (w), 1459 (w), 1440 (s), 1316 (m), 1249 (m), 1151(w), 1093 (m), 949 (w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
18% | With sodium hydroxide In water at 140℃; for 72h; High pressure; | 2.7. Synthesis of complex [Zn(H4bmt)(2, 2′-bipy)]n (5) General procedure: H6bmt (0.05mmol, 0.0179 g), 2, 2′-bipy (0.152mmol, 0.0238 g),Zn(NO3)2·6H2O (0.103mmol, 0.03 g) and 3mL water were mixed in 10mL vial. Then, 50 μL 1 mol/L NaOH was added. The hydrothermal reaction was performed on the same conditions with 1. Colourless crystals were collected and washed with deionized water. Yield: 41.59mg (58%, based on Zn). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | With hydrogen fluoride; urea In water at 80℃; for 96h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62% | With terephthalic acid; hydrogen fluoride In water at 160℃; for 96h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With hydrogen fluoride In water at 160℃; for 96h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium hydroxide at 100℃; for 48h; Autoclave; | 1 Example 1 A cobalt phosphonate, its preparation method comprises: adding 0.72g H6bmt, 0.46g 4,4′-bipyridine and 0.6g Co(OAc)2·4H2O to 30mL deionized water, stirring and adding 60 μL 1mol / L NaOH solution. Then place it in an autoclave at 100 for 48h at constant temperature. after cooling to room temperature, crystals precipitated, and the crystals were washed with deionized water multiple times to obtain cobalt phosphonates. the cobalt phosphonate is a pink lumpy crystal. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48% | at 140℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | at 140℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96.5 % | In water at 20℃; | 1.S4-3.S4 S4: Synthesis of aluminum (IV) 1,3,5-benzenetrimethylphosphonate Intermediate III (3.60g, 10.00mmol) was dissolved in 20mL of distilled water, aluminum sulfate octadecahydrate (7.33g, 11.00mmol) was dissolved in 50mL of distilled water, the above two solutions were transferred to a 250mL reaction bottle, and then reacted at room temperature, The reaction solution gradually changed from colorless and transparent to white emulsion. After 3 hours of reaction, the stirring was stopped, suction filtered, washed with 80 mL of distilled water, and dried in a vacuum oven at 60°C for 8 hours to obtain 3.94 g of white powder with a yield of 96.5%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: N-Bromosuccinimide; dibenzoyl peroxide / tetrachloromethane / 12 h / 20 °C 2: 12 h / 150 °C / Inert atmosphere 3: hydrogenchloride / water / 20 h / 110 °C |