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CAS No. : | 4671-77-6 | MDL No. : | MFCD01631212 |
Formula : | C4H12O6P2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | JKTORXLUQLQJCM-UHFFFAOYSA-N |
M.W : | 218.08 | Pubchem ID : | 437082 |
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 |
---|---|---|
With hydrogenchloride | ||
With hydrogenchloride | ||
7.4 g | With hydrogenchloride; water Reflux; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
(i) (heating), (ii) PCl5; Multistep reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With dihydrogen peroxide |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Cl2-P(O)-(CH2)4-(O)PCl2, H2O2; | ||
Cl2-P(O)-(CH2)4-(O)PCl2, Cl2, H2O; | ||
1,4-Dibrom-butan, 1. Na-diethylphosphit, Ae., Rueckfluss, -> Ester, 2. konz.HCl, Hydrolyse; |
1,4-Dibrom-butan, 1. K-diethylphosphit, Ae., Rueckfluss, -> Ester, 2. konz.HCl, Hydrolyse; | ||
1,4-Dibrom-butan, 1. Na-diethylphosphit, Diglym, Rueckfluss, -> Ester, 2. konz.HCl, Hydrolyse; | ||
1,4-Dibrom-butan, 1. K-diethylphosphit, Diglym, Rueckfluss, -> Ester, 2. konz.HCl, Hydrolyse; | ||
aus dem Ester; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
57% | With dicyclohexyl-carbodiimide In tetrahydrofuran for 75h; Heating; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water the aq. soln. of Zn(ClO4)*6H2O is added to the stirred acidic soln. (aq. HCl) of the bisphosphonic acid, to which 2 M NaOH is subsequently added; product is filtd., washed with water/ethanol, dried in air; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
25% | In water High Pressure; hydrothermal; at 180°C for 39 h, Cu:Mo:bpy:acid:H2O=1.0:1.7:1.9:2.5:3760; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
30% | In water soln. CuSO4*5H2O, Na2MoO4*2H2O, 2,2'-bipyridine, 1,4-butylene diphosphonic acid, and water was heated to 180°C for 39 h; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
36% | With NaOH In water; dimethyl sulfoxide to aq. soln. of NiCl2*6H2O and 1,4-butylenediphosphonic acid added aq. NaOH and then added DMSO with vigorous stirring; soln. filtered; compd. crystd. for 40 d; crystals filtered and dried at ambient temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
6.9% | In sodium hydroxide; water; dimethyl sulfoxide aq. NaOH; to aq. soln. of CuCl2*6H2O and 1,4-butylenediphosphonic acid added DMSO and then added aq. NaOH; soln. filtered and left at ambient temp. for 40d; crystals filtered, washed with water, dried at ambient temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
10% | With NaOH In water; isopropyl alcohol to aq. soln. of NiCl2*6H2O and 1,4-butylenediphosphonic acid added aq. NaOH; soln. filtered and layered with isopropyl alc. and left at ambient temp. for 110 d; crystals filtered, washed with water, ethanol, ether and dried at ambient temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | In water hydrothermal reaction, Cu:V:1,10-phen:P-compd:H2O molar ratio was 1:1:1:2:556, 120 °C for 72 h; washing with H2O, drying at ambient temp., elem. anal.; some amt. of unknown product was also formed; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With HF In water by the react. of MoO3 (1.112 mmol), Cu-contg. compd. (0.451 mmol), ligand (0.224 mmol), H2PO3(CH2)4PO3H2 (0.440 mmol), H2O (557 mmol) and HF washeated at 150°C for 72 h; initial pH 1.5; final pH 1.0; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | In water High Pressure; hydrothermal synthesis; mixt. of Co acetate, NaVO3, phenanthroline, 1,4-butylenediphosphonic acid, and H2O (molar ratio: 1:2:2:2:556) heated at 120°C for 72 h; cooled to room temp., ppt. isolated; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | In water High Pressure; Co(OAC)2*4H2O, Na2MoO4, MoO3, 1,10-phenanthroline, P compd. and distd. water homogenized and heated at 180°C for 72 h in Teflon-lined stainless steel vessel under autogenous pressure; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
25% | With aq. NaOH In water Co, P and org. compds. dissolved in water, pH adjusted to 4.13 with 1 M aq. NaOH; filtered, dried in desiccator filled with silica gel for 3 mo, cryst. washed with water, dried at ambient temp., elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With NaOH In water; dimethyl sulfoxide to aq. soln. of CoSO4*7H2O and 1,4-butylenediphosphonic acid added aq. NaOH and then added DMSO with vigorous stirring; compd. crystd. after 70 d; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
18% | With urea In sodium hydroxide; water aq. NaOH; to aq. soln. of ZnSO4*7H2O and 1,4-butylenediphosphonic acid added aq. NaOH; urea added to soln. and dissolved; soln. filtered and left at 55°C for 24 h; crystals filtered, washed with water and dried at ambient temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In hydrogenchloride; water; dimethyl sulfoxide ZnCl2, 1,4-butylenediphosphonic acid and small amt. of aq. HCl mixed in water and DMSO added to soln. with stirring then aq. NaOH added to soln.; soln. filtered and left at ambient environment for 6 mo; crystals filtered, washed with water and dried at ambient temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
20% | With HF In water High Pressure; under conventional hydrothermal conditions; Mo compd., Ni salt, ligand, H2PO3(CH2)4PO3H2, H2O (molar ratio 0.47:1.29:1.00:2.03:2482) and HF heated in stainless steel container at 200°C for 96 h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | With HF In water High Pressure; under conventional hydrothermal conditions; Mo compd., Ni salt, ligand, H2PO3(CH2)4PO3H2, H2O (molar ratio 0.72:2.01:1.00:2.01:2543) and HF stirred briefly; heated in stainless steel container at 200°C for 96 h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With HF In water High Pressure; mixt. Na3VO4, CuO, bisterpy, H2O3P(CH2)4PO3H2, water, and HF (5.05:2.06:1.00:5.11:4002:47.50) (pH 2.0) was heated to 120°C for 72 h in poly(tetrafluoroethylene) lined stainless steel autoclave under autogenouspressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
20% | In water High Pressure; mixt. V2O5, Cu(OAc)2*H2O, bisterpy, 1,4-butylenediphosphonic acid, waterand hydrofluoric acid (1.94:1.94:1.00:3.80:3800:39.8) was heated in pol y(tetrafluoroethylene) lined stainless steel container to 200°C for 72 h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
5% | In water High Pressure; soln. CuSO4*5H2O, Na3VO4, terpy and 1,4-butylene diphosphonic acid in water was heated in polytetrafluoroethylene-lined stainless steel autoclave to 120°C for 4 days; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | In water High Pressure; soln. of V2O5 (0.99 equiv.), P acid (1 equiv.), H2O (297 equiv.), diamine (1.35 equiv.) and HF (7.75 equiv.) was stirred before heating to 180°C for 96 h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | With HF In water High Pressure; stainless steel container, autogenous pressure, a soln. of V2O5, phosphonic acid, H2O, diamine and HF (1.92:1.00:1459:3.08:15.2 mole ratio) was stirred briefly before heating to 180°C for 96 h with initial andfinal pH values 3.0 and 3.0; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | With HF In water High Pressure; stainless steel container, autogenous pressure, a soln. of NH4VO3, phosphonic acid, H2O and HF (0.95:1.00:557:9.0 mole ratio) was stirred briefly before heating to 200°C for 96 h with initial and final pH values 1.5 and 2.0; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | With H2N(CH2)4)NH2*2HCl; (CH3)4NBr; NaF In water; acetic acid High Pressure; mixt. of Zn acetate, diphosphonic acid, H2N(CH2)4NH2*2HCl, Me4NBR, NaF, AcOH and water in molar ratio of 1:2:2:2:8:210:440 heated at 180°C for 72 h; allowed to cool slowly to ambient temp., crystals filtered off, washed with water, dried at ambient temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water; acetone contacting ZrPO4O2P(OH)2*2H2O twice with water/acetone soln. of H2O3PC3H7 (80°C, each contact 10 d), maintaining solid in a hydrothermal bomb containing oxygen free water soln. of butyldiphosphonic acid (3 d, 60°C); |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | With HCl In water High Pressure; Cu compd. (0.52 mmol), bpy (0.52 mmol), and P compd. (0.30 mmol) in water, 3 drops of HCl added, briefly stirred, heated at 200°C for 48 h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
35% | In water; acetic acid High Pressure; mixt. MoO3, Co(OAc)2*4H2O, tetra-2-pyridylpyrazine, H2PO3(CH2)4PO3H2, concd. AcOH and water (4.90:1.01:1.00:2.01:2511) was heated at 200°C for 96 h in poly(tetrafluoroethylene)-lined stainless steel container; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62% | With HF In hydrogen fluoride aq. HF; High Pressure; adjusting pH of 6.1:1.9:1:2 mixt. of molybdenum trioxide, copper acetate, bipyrimidine and phosphonic acid deriv. in water to 2 by aq. HF, stirring, heating at 120°C for 96 h; isolation of crystals, elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
55% | Stage #1: 1,4-dibromo-butane; triethyl phosphite for 0.0833333h; Microwave irradiation; Stage #2: With water; hydrogen bromide for 0.0833333h; Microwave irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | With HF In water High Pressure; Cu-compd., MoO3, P-compd., diamine-compd. in H2O with HF stirred for 15 min before heating to 100°C for 48 h, cooled to room temp.; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
38% | With HF In water High Pressure; Cu-compd., MoO3, P-compd., diamine-compd. in H2O with HF stirred brieflybefore heating to 100°C for 48 h; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With acetic acid |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1: 50% 2: 30% | at 150℃; for 48h; High pressure; | 2 2.2 Synthesis of [{Cu2(bisterpy)(H2O)}Mo5O15{O3P(CH2)4PO3}]·4.5H2O (1·4.5H2O) and [{Cu2(bisterpy)(H2O)2}Mo2F6O4{HO3P(CH2)4PO3H}] (6) A solution of cupric acetate (0.045 g, 0.2263 mmol), molybdenum(VI) oxide (0.087 g, 0.6034 mmol), bisterpy (0.050 g, 0.1078 mmol), 1,4-butylenediphosphonic acid (0.059 g, 0.2694 mmol), H2O (10.00 g, 556 mmol), and HF (0.300 mL, 17.24 mmol) with the mole ratio 2.10:5.60:1.00:2.50:5157.70:159.93 was stirred briefly before heating to 150 °C for 48 h with initial and final pH values of 1.5 and 1.0, respectively. Blue and green crystals were isolated in 30% and 50% yield, respectively, that were suitable for X-ray diffraction. IR (KBr pellet, cm-1): 1·4.5H2O: 3423(m), 1606(m), 1561(m), 1476(m), 1409(m), 1248(w), 1159(w), 952(m), 912(s), 793(m), 671(w), 580(m); 6·2H2O: 3447(m), 1607(m), 1552(w), 1476(m), 1409(m), 1248(w), 1158(w), 949(m), 912(s), 793(m), 671(w), 580(m). Anal. Calc. for 1, Mo5Cu2P2C34H39N6O26.5: C, 25.1; H, 2.40; N, 5.17. Found: C, 24.7; H, 2.55; N, 5.05%. Anal. Calc. for 6, Mo2Cu2P2C34H34N6O12F6: C, 33.6; H, 2.54; N, 6.92; F, 9.39. Found: C, 33.5; H, 2.61; N, 7.04; F, 9.13%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water at 160℃; for 48h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With acetic acid for 48h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With acetic acid for 336h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
61% | In water at 160℃; for 48h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
41% | In water at 180℃; for 72h; Autoclave; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With perchloric acid In methanol; water; butan-1-ol Schlenk technique; | 2.2 Single crystal growth General procedure: For Hg2(HO3P(C6H4)PO3H)(2) compound, Hg2(ClO4)2·4H2O (0.2254g, 0.335mmol), was dissolved in 2mL of concentrated perchloric acid and later diluted to 10mL with distilled water. This acidic aqueous solution was layered with a homogenous mixture of 10mL n-butanol and 1.5mL water. On its top, a 5mL methanol solution of 1,4-phenylenebisphosphonic acid (0.0798g, 0.335mmol) was added slowly using a syringe. Crystals of compound 2 were formed at the butanol-water interphase as well as at the inner walls of Schlenk tube in butanol layer. After a period of two weeks, the aqueous acidic solution was syringed out and the crystals were filtered and air-dried. (0014) The crystal growth experiments for the remaining four mercurous diphosphonates, 3, 4, 6 and 7, were carried out in a similar way. The respective quantities of Hg2(ClO4)2·4H2O and the corresponding phosphonic/bisphosphonic acid employed were 0.1212g (0.180mmol) and 0.0566g (0.180mmol) for compound 3, 0.1372g (0.204mmol) and 0.0445g (0.204mmol) for compound 4, 0.124g (0.184mmol) and 0.0349g (0.184mmol) for compound 6 and 0.152g (0.226mmol) and 0.0461g (0.226mmol) for compound 7. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48% | In water at 200℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | In water at 200℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | In water at 200℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48% | In water at 200℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
31% | Stage #1: Na9[A-α-PW9O34]*7H2O; manganese(III) triacetate dihydrate In aq. acetate buffer at 20℃; for 1h; Stage #2: 1,4-butylenediphosphonic acid In aq. acetate buffer for 2h; Stage #3: N,N-dimethylammonium chloride In aq. acetate buffer |