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[ CAS No. 1939-36-2 ] {[proInfo.proName]}

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3d Animation Molecule Structure of 1939-36-2
Chemical Structure| 1939-36-2
Chemical Structure| 1939-36-2
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Product Details of [ 1939-36-2 ]

CAS No. :1939-36-2 MDL No. :MFCD00210039
Formula : C11H18N2O8 Boiling Point : -
Linear Structure Formula :- InChI Key :DMQQXDPCRUGSQB-UHFFFAOYSA-N
M.W : 306.27 Pubchem ID :80296
Synonyms :

Safety of [ 1939-36-2 ]

Signal Word:Danger Class:8
Precautionary Statements:P264-P270-P280-P301+P312-P305+P351+P338-P310-P330-P501 UN#:1759
Hazard Statements:H302-H318 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 1939-36-2 ]

* 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.

  • Downstream synthetic route of [ 1939-36-2 ]

[ 1939-36-2 ] Synthesis Path-Downstream   1~50

  • 1
  • [ 1939-36-2 ]
  • C11H18N2O10 [ No CAS ]
YieldReaction ConditionsOperation in experiment
72% With dihydrogen peroxide In acetic acid at 20℃;
  • 2
  • [ 1939-36-2 ]
  • [ 7718-98-1 ]
  • Na(1+)*{V((O2CCH2)2NCH2CH2CH2N(CH2CO2)2)}(1-)*3H2O=Na{V((O2CCH2)2NCH2CH2CH2N(CH2CO2)2)}*3H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
54% With Na2CO3 In water under N2, suspn. of H4trdta was neutralized with Na2CO3, addn. of VCl3, stirred at room temp. for 30 min;; filtration, washed with water, ethanol, ether, dried; elem. anal.;;
  • 3
  • [ 1939-36-2 ]
  • [ 7718-98-1 ]
  • K(1+)*{V((O2CCH2)2NCH2CH2CH2N(CH2CO2)2)}(1-)*4H2O=K{V((O2CCH2)2NCH2CH2CH2N(CH2CO2)2)}*4H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
43% With K2CO3 In water under N2, suspn. of H4trdta was neutralized with K2CO3, addn. of VCl3, stirred at room temp. for 30 min;; filtration, washed with water, ethanol, ether, dried; elem. anal.;;
  • 4
  • hexamminechromium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • hexaamminechromium(III) sodium propylenediaminetetraacetate trihydrate [ No CAS ]
YieldReaction ConditionsOperation in experiment
With sodium hydroxide In water addition of soln. of H4pdta in aq. NaOH (molar ratio 5:2) to a soln. ofcomplex (complex:H4pdta molar ratio 1:1); addition of ethanol, cooling for a few days in refrigerator, recrystn. (water); elem. anal.;
  • 5
  • [ 1939-36-2 ]
  • W3SO3(H2O)9(4+)*4Cl(1-)=(W3SO3(H2O)9)Cl4 [ No CAS ]
  • Na4((W3SO3)2(PDTA)3)*11H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
45.6% In water; N,N-dimethyl-formamide to soln. (W3SO3(H2O)9)Cl4 in DMF was added H4PDTA and refluxed for 4 h, solid was filtered, dissolved in water and passed through cation exchange column (Na+); eluate was evapd. to dryness under vac., residue was dissolved in water and loaded on Sephadex G-25 column, aq. eluate was concd. to dryness in vacuo; elem. anal.;
  • 6
  • ammonium heptamolybdate tetrahydrate [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • [(NH4)8(Mo(VI)10O32(1,3-diaminopropanetetraacetate))(H2O)30] [ No CAS ]
YieldReaction ConditionsOperation in experiment
19% With HCl In water (NH4)6Mo7O24*7H2O and 1,3-diaminopropanetetraacetic acid dissolved in H2O upon stirring; pH adjusted to 3.7-3.8 (4 M HCl); refluxed at 70°C for ca. 1.5 h; cooled to room temp.; soln. filtered; crystd. by slow evapn. at room temp. for ca. 1 mo; elem.anal.;
  • 7
  • [ 1939-36-2 ]
  • potassium hydroxide [ No CAS ]
  • [ 7646-85-7 ]
  • K2[ZnCl2(1,3-propanediaminetetraacetic acid(-2H)ZnCl2] [ No CAS ]
YieldReaction ConditionsOperation in experiment
80% In water H4pdta (1 mmol) added to aq. soln. of ZnCl2 (1 mmol), pH 1.5 (KOH), mixt. stirred for 2 h at room temp.; cystd. on slow evapn., filtered off, washed (EtOH), dried in air, elem. anal.;
78% In water H4pdta (1 mmol) added to aq. soln. of ZnCl2 (2 mmol), pH 1.5 (KOH), mixt. stirred for 2 h at room temp.; cystd. on slow evapn., filtered off, washed (EtOH), dried in air, elem. anal.;
  • 8
  • [ 1939-36-2 ]
  • [ 106-94-5 ]
  • [ 107-21-1 ]
  • [ 95-54-5 ]
  • [ 1299486-28-4 ]
YieldReaction ConditionsOperation in experiment
Stage #1: 1,3-propanediaminetetraacetatic acid; ethylene glycol; 1,2-diamino-benzene at 200℃; for 22h; Stage #2: propyl bromide With potassium hydroxide In dimethyl sulfoxide at 20℃; for 3h; 4 Synthesis Example 4The above-described ligand represented by formula (B-10) was synthesized according to the description in the Journal of American Chemical Society 104, 3607 to 3617 (1982) and in Tetrahedron Letter, 29, 3033 to 3036. A mixture of 1,2-diaminobenzene, 1,3-propane-N,N,N',N'-tetraacetic acid, and ethylene glycol was reacted by heating at 200° C. for 22 hours. Then, the resultant product and 1-bromopropane were reacted for 3 hours in dimethyl sulfoxide solution at room temperature in the presence of potassium hydroxide, to obtain the above-described ligand represented by formula (B-10).
  • 9
  • zinc(II) nitrate hexahydrate [ No CAS ]
  • [ 1939-36-2 ]
  • [Zn(nitrato)2(H2O)(1,3-propanediaminetetraacetatic acid)]n [ No CAS ]
YieldReaction ConditionsOperation in experiment
62% With hydrogenchloride In water at 20℃; for 2h; 2.1 Preparation of [Zn(NO3)2(H2O)(1,3-H4pdta)]n (1) 1,3-Propanediaminetetraacetic acid (3.1 g, 10 mmol) was added to a stirred solution of Zn(NO3)2·6H2O (3.0 g, 10 mmol) in water (30 mL). The mixture was stirred for 2 h at room temperature. The pH value of the solution was adjusted to 1.0 with diluted hydrochloric acid. The solution was left to evaporate for several days to give a colorless crystalline product. Compound 1 was isolated by filtration, washed with ethanol and dried in air. Yield: 3.2 g (62%). IR (KBr, cm-1): 3569, 3427m, br, 3162s, 2973m, 1907w, 1727s, 1600vs, 1478vs, 1406vs, 1383vs, 1358s, 1313vs, 1212s, 1086m, 1035m, 990m, 963w, 901m, 815w, 756w, 688w, 610w, 534w, 454w. Anal. Calc. for C11H20N4O15Zn: C, 25.7; H, 3.9; N, 10.9. Found: C, 25.5; H, 4.1; N, 10.8%.
  • 10
  • [ 109-76-2 ]
  • [ 79-11-8 ]
  • [ 1939-36-2 ]
  • [ 57119-37-6 ]
  • [ 60972-23-8 ]
YieldReaction ConditionsOperation in experiment
With calcium oxide In water at 50 - 70℃; for 6.5h; Preparation of condensation mixture containing 1,3-propanediamine-N,N,N′-triacetic acid, H31,3-pd3a 1,3-propanediamine-N,N,N′-triacetic acid, H31,3-pd3a was prepared by the method described elsewhere [7]. Monochloroacetic acid (11.5 g, 120 mmol) was dissolved in 42 ml of demineralized water and 4.7 g (84 mmol) calcium oxide was added to the solution. The pH rose from 1.0 to 11.2. Subsequently, 3.11 g (42 mmol) of 1,3-propanediamine was added in 10 min. The temperature was kept at about 50 °C without additional heating. After 1 h the temperature was increased to 70 °C and the resulting mixture was left for additional 5.5 h. During the entire reaction, the pH was kept constant at 7.5-8.0 by the addition of calcium oxide. At the end of the reaction, a total of 1.9 g (34 mmol) of calcium oxide was added. The reaction mixture was filtered warm over a glass filter to remove the excess of calcium hydroxide. The reaction mixture (volume 50 ml) contains 1,3-pd3a (50%), 1,3-pdta (18%) i 1,3-pdda (23%) ligands. This was checked by means of chromatography of copper(II) complexes with above mixture.
  • 11
  • [ 1939-36-2 ]
  • lanthanide(III)chloride heptahydrate [ No CAS ]
  • [ 7732-18-5 ]
  • {La(H2O)4[La(1,3-propanediaminetetraacetate)(H2O)]3}n·12nH2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
57% Stage #1: 1,3-propanediaminetetraacetatic acid With ammonium hydroxide In water Stage #2: lanthanide(III)chloride heptahydrate; water With ammonium hydroxide at 70℃; for 20h;
  • 12
  • [ 1336-21-6 ]
  • [ 1939-36-2 ]
  • lanthanide(III)chloride heptahydrate [ No CAS ]
  • (NH4)2[La2(1,3-propanediaminetetraacetato)2(H2O)4]·8H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
61% Stage #1: 1,3-propanediaminetetraacetatic acid; lanthanide(III)chloride heptahydrate In water for 1.5h; Stage #2: ammonium hydroxide In water at 70℃; for 12h;
  • 13
  • [ 1939-36-2 ]
  • lanthanide(III)chloride heptahydrate [ No CAS ]
  • potassium hydroxide [ No CAS ]
  • K2[La2(1,3-propanediaminetetraacetato)2(H2O)4]·11H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
76% Stage #1: 1,3-propanediaminetetraacetatic acid; lanthanide(III)chloride heptahydrate In water for 1.5h; Stage #2: potassium hydroxide In water at 70℃; for 12h;
  • 14
  • [ 7790-86-5 ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H17N2O8(1-)*8H2O*2Cl(1-)*Ce(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide for 0.5h; Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) General procedure: Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) KOH (1.12 g, 20.0 mmol) and 1,3-propanediaminetetraacetic acid (6.2 g, 20.0 mmol) were dissolved in water (75 mL) and stirred for several minutes. LaCl3·7H2O (7.4 g, 20.0 mmol) was added. The pH value was 1.5-2.0. The solution was stirred for half an hour and then standing in air. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with cold water and ethanol, and dried in the air. The yield of 1 was 92% (12.1 g). Anal. Found (calcd. for C11H33N2O16Cl2La): C, 19.7 (20.0); H, 5.1 (5.0); N, 4.0 (4.2). IR (KBr disk, /cm-1): 3404s, 3019s, νas(CO2H), 1739s, 1707s, νas(CO2), 1616s; νs(CO2), 1413s; 1342m, 1254m, 1197m, 1119w, 1067m, 971w, 907w, 883m, 851w, 700m, 533w, 477w.
  • 15
  • [ 7790-86-5 ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H16N2O8(2-)*4H2O*Cl(1-)*Ce(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 70℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 16
  • [ 7790-86-5 ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H15N2O8(3-)*H2O*Ce(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 180℃; for 60h; One pot synthesis of [La(1,3-Hpdta)]n·nH2O (15) General procedure: KOH (0.11-0.17g, 2.0-3.0mmol), 1,3-propanediaminetetraacetic acid (0.31g, 1.0mmol), water (15mL) and LaCl3·7H2O (0.37g, 1.0mmol) were sealed into a 25mL teflon-lined stainless steel vessel, heated at 180°C for 60h, and then (40h) cooled to room temperature. Colorless crystalline materials were separated. The solids were washed with water, and dried in air. The yield of 15 was 55% (0.25g). Anal. Found (calcd. for C11H17N2O9La): C, 28.8 (28.7); H, 3.9 (3.7); N, 6.1 (6.1). One pot synthesis of complexes 16-20 were similar to that of 15.
  • 17
  • praseodymium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H17N2O8(1-)*8H2O*2Cl(1-)*Pr(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide for 0.5h; Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) General procedure: Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) KOH (1.12 g, 20.0 mmol) and 1,3-propanediaminetetraacetic acid (6.2 g, 20.0 mmol) were dissolved in water (75 mL) and stirred for several minutes. LaCl3·7H2O (7.4 g, 20.0 mmol) was added. The pH value was 1.5-2.0. The solution was stirred for half an hour and then standing in air. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with cold water and ethanol, and dried in the air. The yield of 1 was 92% (12.1 g). Anal. Found (calcd. for C11H33N2O16Cl2La): C, 19.7 (20.0); H, 5.1 (5.0); N, 4.0 (4.2). IR (KBr disk, /cm-1): 3404s, 3019s, νas(CO2H), 1739s, 1707s, νas(CO2), 1616s; νs(CO2), 1413s; 1342m, 1254m, 1197m, 1119w, 1067m, 971w, 907w, 883m, 851w, 700m, 533w, 477w.
  • 18
  • praseodymium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H16N2O8(2-)*4H2O*Cl(1-)*Pr(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 70℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 19
  • praseodymium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H15N2O8(3-)*H2O*Pr(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 180℃; for 60h; One pot synthesis of [La(1,3-Hpdta)]n·nH2O (15) General procedure: KOH (0.11-0.17g, 2.0-3.0mmol), 1,3-propanediaminetetraacetic acid (0.31g, 1.0mmol), water (15mL) and LaCl3·7H2O (0.37g, 1.0mmol) were sealed into a 25mL teflon-lined stainless steel vessel, heated at 180°C for 60h, and then (40h) cooled to room temperature. Colorless crystalline materials were separated. The solids were washed with water, and dried in air. The yield of 15 was 55% (0.25g). Anal. Found (calcd. for C11H17N2O9La): C, 28.8 (28.7); H, 3.9 (3.7); N, 6.1 (6.1). One pot synthesis of complexes 16-20 were similar to that of 15.
  • 20
  • neodymium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H17N2O8(1-)*8H2O*2Cl(1-)*Nd(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide for 0.5h; Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) General procedure: Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) KOH (1.12 g, 20.0 mmol) and 1,3-propanediaminetetraacetic acid (6.2 g, 20.0 mmol) were dissolved in water (75 mL) and stirred for several minutes. LaCl3·7H2O (7.4 g, 20.0 mmol) was added. The pH value was 1.5-2.0. The solution was stirred for half an hour and then standing in air. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with cold water and ethanol, and dried in the air. The yield of 1 was 92% (12.1 g). Anal. Found (calcd. for C11H33N2O16Cl2La): C, 19.7 (20.0); H, 5.1 (5.0); N, 4.0 (4.2). IR (KBr disk, /cm-1): 3404s, 3019s, νas(CO2H), 1739s, 1707s, νas(CO2), 1616s; νs(CO2), 1413s; 1342m, 1254m, 1197m, 1119w, 1067m, 971w, 907w, 883m, 851w, 700m, 533w, 477w.
  • 21
  • neodymium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H16N2O8(2-)*4H2O*Cl(1-)*Nd(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 70℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 22
  • neodymium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H15N2O8(3-)*H2O*Nd(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 180℃; for 60h; One pot synthesis of [La(1,3-Hpdta)]n·nH2O (15) General procedure: KOH (0.11-0.17g, 2.0-3.0mmol), 1,3-propanediaminetetraacetic acid (0.31g, 1.0mmol), water (15mL) and LaCl3·7H2O (0.37g, 1.0mmol) were sealed into a 25mL teflon-lined stainless steel vessel, heated at 180°C for 60h, and then (40h) cooled to room temperature. Colorless crystalline materials were separated. The solids were washed with water, and dried in air. The yield of 15 was 55% (0.25g). Anal. Found (calcd. for C11H17N2O9La): C, 28.8 (28.7); H, 3.9 (3.7); N, 6.1 (6.1). One pot synthesis of complexes 16-20 were similar to that of 15.
  • 23
  • samarium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H17N2O8(1-)*8H2O*2Cl(1-)*Sm(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide for 0.5h; Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) General procedure: Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) KOH (1.12 g, 20.0 mmol) and 1,3-propanediaminetetraacetic acid (6.2 g, 20.0 mmol) were dissolved in water (75 mL) and stirred for several minutes. LaCl3·7H2O (7.4 g, 20.0 mmol) was added. The pH value was 1.5-2.0. The solution was stirred for half an hour and then standing in air. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with cold water and ethanol, and dried in the air. The yield of 1 was 92% (12.1 g). Anal. Found (calcd. for C11H33N2O16Cl2La): C, 19.7 (20.0); H, 5.1 (5.0); N, 4.0 (4.2). IR (KBr disk, /cm-1): 3404s, 3019s, νas(CO2H), 1739s, 1707s, νas(CO2), 1616s; νs(CO2), 1413s; 1342m, 1254m, 1197m, 1119w, 1067m, 971w, 907w, 883m, 851w, 700m, 533w, 477w.
  • 24
  • samarium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H16N2O8(2-)*5H2O*Cl(1-)*Sm(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 20℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 25
  • samarium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H16N2O8(2-)*4H2O*Cl(1-)*Sm(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 70℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 26
  • samarium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H15N2O8(3-)*5H2O*Sm(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 180℃; for 60h; One pot synthesis of [La(1,3-Hpdta)]n·nH2O (15) General procedure: KOH (0.11-0.17g, 2.0-3.0mmol), 1,3-propanediaminetetraacetic acid (0.31g, 1.0mmol), water (15mL) and LaCl3·7H2O (0.37g, 1.0mmol) were sealed into a 25mL teflon-lined stainless steel vessel, heated at 180°C for 60h, and then (40h) cooled to room temperature. Colorless crystalline materials were separated. The solids were washed with water, and dried in air. The yield of 15 was 55% (0.25g). Anal. Found (calcd. for C11H17N2O9La): C, 28.8 (28.7); H, 3.9 (3.7); N, 6.1 (6.1). One pot synthesis of complexes 16-20 were similar to that of 15.
  • 27
  • gadolinium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H16N2O8(2-)*5H2O*Cl(1-)*Gd(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 20℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 28
  • gadolinium(III) chloride [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H16N2O8(2-)*4H2O*Cl(1-)*Gd(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide at 70℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 29
  • [ 1939-36-2 ]
  • EuCl3*7H2O [ No CAS ]
  • C11H16N2O8(2-)*4H2O*Cl(1-)*Eu(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
78% With potassium hydroxide In water at 70℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: KOH (0.22g, 4.0mmol) and 1,3-propanediaminetetraacetic acid (0.62g, 2.0mmol) were dissolved in water (15mL). LaCl3·7H2O (0.74g, 2.0mmol) was added. The solution was stirred for half an hour and then standing in 70°C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1). One pot synthesis of complexes 9-14 were similar to that of 8. Synthesis of [Ln(1,3-H2pdta)(H2O)3]n·Cln·2nH2O [Ln=Sm, 6; Gd, 7] were similar to that of 8, but standing in room temperature.
  • 30
  • [ 1939-36-2 ]
  • EuCl3*7H2O [ No CAS ]
  • C11H15N2O8(3-)*5H2O*Eu(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide In water at 180℃; for 60h; One pot synthesis of [La(1,3-Hpdta)]n·nH2O (15) General procedure: KOH (0.11-0.17g, 2.0-3.0mmol), 1,3-propanediaminetetraacetic acid (0.31g, 1.0mmol), water (15mL) and LaCl3·7H2O (0.37g, 1.0mmol) were sealed into a 25mL teflon-lined stainless steel vessel, heated at 180°C for 60h, and then (40h) cooled to room temperature. Colorless crystalline materials were separated. The solids were washed with water, and dried in air. The yield of 15 was 55% (0.25g). Anal. Found (calcd. for C11H17N2O9La): C, 28.8 (28.7); H, 3.9 (3.7); N, 6.1 (6.1). One pot synthesis of complexes 16-20 were similar to that of 15.
  • 31
  • [ 1939-36-2 ]
  • lanthanide(III)chloride heptahydrate [ No CAS ]
  • C11H17N2O8(1-)*La(3+)*8H2O*2Cl(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
92% With potassium hydroxide In water for 0.5h; Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) General procedure: Preparation of [La(1,3-H3pdta)(H2O)4]n·2Cln·3nH2O (1) KOH (1.12 g, 20.0 mmol) and 1,3-propanediaminetetraacetic acid (6.2 g, 20.0 mmol) were dissolved in water (75 mL) and stirred for several minutes. LaCl3·7H2O (7.4 g, 20.0 mmol) was added. The pH value was 1.5-2.0. The solution was stirred for half an hour and then standing in air. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with cold water and ethanol, and dried in the air. The yield of 1 was 92% (12.1 g). Anal. Found (calcd. for C11H33N2O16Cl2La): C, 19.7 (20.0); H, 5.1 (5.0); N, 4.0 (4.2). IR (KBr disk, /cm-1): 3404s, 3019s, νas(CO2H), 1739s, 1707s, νas(CO2), 1616s; νs(CO2), 1413s; 1342m, 1254m, 1197m, 1119w, 1067m, 971w, 907w, 883m, 851w, 700m, 533w, 477w.
  • 32
  • [ 1939-36-2 ]
  • lanthanide(III)chloride heptahydrate [ No CAS ]
  • C11H16N2O8(2-)*4H2O*Cl(1-)*La(3+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
75% With potassium hydroxide In water at 70℃; One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) General procedure: One pot synthesis of [La(1,3-H2pdta)(H2O)2]n·Cln·2nH2O (8) KOH (0.22 g, 4.0 mmol) and 1,3-propanediaminetetraacetic acid (0.62 g, 2.0 mmol) were dissolved in water (15 mL). LaCl3·7H2O (0.74 g, 2.0 mmol) was added. The solution was stirred for half an hour and then standing in 70 °C. Colorless crystalline materials were separated after evaporation of the solution. The solids were washed with water and ethanol, and dried in the air. The yield of 8 was 75% (0.83 g). Anal. Found (calcd. for C11H24N2O12ClLa): C, 23.8 (24.0); H, 4.5 (4.4); N, 5.0 (5.1).
  • 33
  • [ 1939-36-2 ]
  • lanthanide(III)chloride heptahydrate [ No CAS ]
  • C11H15N2O8(3-)*La(3+)*H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
55% With potassium hydroxide In water at 180℃; for 60h; One pot synthesis of [La(1,3-Hpdta)]n·nH2O (15) General procedure: KOH (0.11-0.17g, 2.0-3.0mmol), 1,3-propanediaminetetraacetic acid (0.31g, 1.0mmol), water (15mL) and LaCl3·7H2O (0.37g, 1.0mmol) were sealed into a 25mL teflon-lined stainless steel vessel, heated at 180°C for 60h, and then (40h) cooled to room temperature. Colorless crystalline materials were separated. The solids were washed with water, and dried in air. The yield of 15 was 55% (0.25g). Anal. Found (calcd. for C11H17N2O9La): C, 28.8 (28.7); H, 3.9 (3.7); N, 6.1 (6.1). One pot synthesis of complexes 16-20 were similar to that of 15.
  • 34
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • copper dichloride [ No CAS ]
  • [Cu4(1,3-pdta)2(H2O)4]·H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
63% With zinc(II) acetate dihydrate at 20℃; for 2h; 2.3 Preparation of [Cu4(1,3-pdta)2(H2O)4]·H2O (3) 1,3-Propanediaminetetraacetic acid (0.62g, 2.0mmol) was added to a stirred solution of CuCl2 (0.52g, 4.0mmol) in water (15mL). Zn(OAc)2·2H2O (4.0mL, 1.0mol/L) was added to the mixture. The solution was stirred for 2h at room temperature and left standing for 4days to give a blue crystalline product of 3. The solid was isolated by filtration, washed with water and ethanol and dried in air. Yield: 0.60g (63%). IR (KBr, cm-1): 3442vs,br, 2961, 2924, 2851, 1591vs, 1454m, 1393s, 1333m, 1264m, 1157w, 1130m, 1096m, 1068w, 995w, 920m, 893w, 744m, 641m, 617m, 512m, 467m, 415m; Anal. Calc. for C22H38Cu4N4O21: C, 27.8; H, 4.0; N, 5.9. Found: C, 27.4; H, 4.4; N, 5.5%.
  • 35
  • [ 1939-36-2 ]
  • copper dichloride [ No CAS ]
  • Cu(2+)*C11H16N2O8(2-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
69% With potassium hydroxide In water at 20℃; for 2h; 2 2.2 Preparation of [Cu(1,3-H2pdta)]n (2) 1,3-Propanediaminetetraacetic acid (0.62 g, 2.0 mmol) was added to a stirred solution of CuCl2 (0.26 g, 2.0 mmol) in water (15 mL). The pH value of the mixture was adjusted to 2.5 by potassium hydroxide (5.0 mol/L). The mixture was stirred for 2 h at room temperature and left standing in 70 °C for 2 days to give a blue crystalline solid of 2. The product was isolated by filtration, washed with water and ethanol and dried in air. Yield: 0.51 g (69%). IR (KBr, cm-1): 3430m,br, 2966s, 2893m, 1725s, 1594vs, 1445s, 1385vs, 1279s, 1224s, 1148m, 1090m, 956w, 910w, 887m, 837m, 750w, 674w, 585w, 559w, 476w, 404m; Anal. Calc. for C11H16N2O8Cu: C, 35.9; H, 4.4; N, 7.6. Found: C, 36.2; H, 4.4; N, 7.6%.
  • 36
  • [ 1939-36-2 ]
  • copper dichloride [ No CAS ]
  • C22H32Cl4Cu4N4O16 [ No CAS ]
YieldReaction ConditionsOperation in experiment
53% With potassium hydroxide In water at 20℃; for 2h; 2.1 Preparation of [Cu4Cl4(1,3-H2pdta)2] (1) 1,3-Propanediaminetetraacetic (0.62 g, 2.0 mmol) was added to a stirred solution of CuCl2 (0.52 g, 4.0 mmol) in water (15 mL). The pH value of the mixture was adjusted to 2.5 by potassium hydroxide (5.0 mol/L). The mixture was stirred for 2 h at room temperature and left standing for 5 days to give a blue crystalline solid of 1. The product was isolated by filtration, washed with water and ethanol and dried in air. Yield: 0.53 g (53%). IR (KBr, cm-1): 3445m,br, 3245s, 2980m, 2952m, 1715s, 1466vs, 1429s, 1344s, 1315m, 1246m, 1193s, 1132m, 1078w, 975w, 949w, 910m, 876m, 753w, 690m, 613m, 483m, 406w; Anal. Calc. for C22H32N4O16Cl4Cu4: C, 26.3; H, 3.2; N, 5.6. Found: C, 26.5; H, 3.4; N, 5.9%.
  • 37
  • lead(II) nitrate [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H14N2O8(4-)*Pb(2+)*3H2O*2H(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
27.6% With potassium hydroxide at 80℃; for 18h; 2.3. Synthesis of [pb(1,3-H2pdta)(H2O)]·2H2O}n (2) 1,3-H4pdta (612mg, 2.0mmol) was dissolved in 10mL water. A solution of Pb(NO3)2 (662mg, 2.0mmol) in 5mL water were added to the above solution. The pH value of the mixture was adjusted to 3.0 with 2.0M KOH. The solution was stirred for 15min at room temperature and warmed at 80°C for 18h and filtered. The filtrate was allowed to evaporate at room temperature. After one week, colorless bulk crystals of 2 were isolated with a yield of 313mg (27.6%). Anal. calcd. for C11H20N2O11Pb (Mr 565.50): C, 23.4; H, 3.6; N, 5.0; found: C, 23.0; H, 3.8; N, 4.9. IR (cm-1): 3440sb, 3021m, 1627s, 1396s, 1322m, 922w, 706w, 540w.
  • 38
  • lead(II) nitrate [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H14N2O8(4-)*2Pb(2+)*2H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
78.4% With potassium hydroxide at 80℃; for 18h; 2.5. Synthesis of [Pb2(1,3-pdta)(H2O)2]n (4) 1,3-H4pdta (306 mg, 1.0 mmol) was dissolved into 10 mL water. A solution of Pb(NO3)2 (331 mg, 1.0 mmol) in 5 mL water were added. The pH value was adjusted to 5.0 with a 2.0 M KOH solution. The mixture was stirred for 15 min at room temperature, and warmed at 80 °C for 18 h. The solution was allowed to evaporate at room temperature. After one week, colorless bulk crystals of 4 were isolated with a yield of 295 mg (78.4%). Anal. calcd. for C11H18N2O10Pb2 (Mr 752.65): C, 17.5; H, 2.4; N, 3.7; found: C, 17.0; H, 2.4; N, 3.6. IR (cm-1): 3441sb, 2925w, 1585s, 1376m, 1111w, 712w, 620w, 538w.
  • 39
  • lead(II) nitrate [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • C11H14N2O8(4-)*2Pb(2+)*8H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
91.5% With potassium hydroxide at 80℃; for 18h; 2.4. Synthesis of [Pb2(1,3-pdta)(H2O)4]·4H2O}n (3) 1,3-H4pdta (612 mg, 2.0 mmol) was dissolved in 10 mL water. A solution of Pb(NO3)2 (331 mg, 1.0 mmol) in 5 mL water were added. The pH value was adjusted to 4.0 with 2.0 M KOH. The mixture was stirred for 15 min at room temperature, and warmed at 80 °C for 18 h. The solution was allowed to evaporate at room temperature. After one day, colorless acicular crystals of 3 were isolated with a yield of 394 mg (91.5% based on lead nitrate). Anal. calcd. for C11H30N2O16Pb2 (Mr 860.75): C, 15.3; H, 3.5; N, 3.3; found: C, 15.0; H, 3.6; N, 3.5. IR (cm-1): 3446sb, 1587s, 1400m, 620w, 483w.
  • 40
  • lead(II) nitrate [ No CAS ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • potassium hydroxide [ No CAS ]
  • 2C11H14N2O8(4-)*2Pb(2+)*6H2O*4K(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
28.1% In methanol at 80℃; for 18h; 2.2. Synthesis of {K4[Pb2(1,3-pdta)2]·6H2O}n (1) 1,3-H4pdta (306 mg, 1.0 mmol) and Pb(NO3)2 (331 mg, 1.0 mmol) was dissolved in water (1.0 mL). The pH value of the mixture was adjusted to 9.0 with 2.0 M KOH. The solution was added with 10 mL methanol and stirred for 15 min at room temperature, and warmed at 80 °C for 18 h. The mixture was allowed to evaporate at room temperature. After one day, colorless acicular crystals of 1 were isolated with a yield of 180 mg (28.1%). Anal. calcd. for C22H40N4O22Pb2K4 (Mr 1283.36): C, 20.6; H, 3.1; N, 4.4; found: C, 20.4; H, 3.1; N, 4.5. IR (cm-1): 3362sb, 2856w, 1583s, 1393s, 1332m, 1256w, 705w, 629w, 557w.
  • 41
  • [ 1939-36-2 ]
  • [ 13477-34-4 ]
  • [ 7732-18-5 ]
  • [Ca(1,3-propylenediaminetetraacetic acid)(NO3)2(water)2] [ No CAS ]
YieldReaction ConditionsOperation in experiment
48.6% With sodium hydroxide at 20 - 80℃; for 18.25h; 2.2. Synthesis of [Ca(1,3-H4pdta)(NO3)2(H2O)2]n (1) 1,3-H4pdta (306 mg, 1.0 mmol) was dissolved in 5 mL water. A solution of Ca(NO3)2 (164 mg, 1.0 mmol) in 2 mL water was added to the above solution, and the pH value of the mixture was adjusted to 2.5 with 2.0 M NaOH. The mixture was stirred for 15 min at room temperature and warmed at 80 C for 18 h. The solution was allowed to evaporate at room temperature. After one week, colorless bulk crystals of 1 were isolated with a yield of 246 mg (48.6%). Anal. calcd. for C11H22N4O16Ca (Mr 506.40): C,26.1; H, 4.3; N, 11.1; found: C, 26.1; H, 3.7; N, 11.3. IR (cm1): 3432sb, 1726vw, 1634 s, 1408m, 1384s, 1260w, 1107w, 902w, 802w,618w.
  • 42
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • calcium chloride [ No CAS ]
  • C11H14N2O8(4-)*Ca(2+)*H2O*2H(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
34.5% With sodium hydroxide In methanol at 20 - 80℃; for 18.25h; 2.3. Synthesis of [Ca(1,3-H2pdta)]n.nH2O (2) 1,3-H4pdta (306 mg, 1.0 mmol) was dissolved in 5 mL water. A solution of CaCl2 (110 mg, 1.0 mmol) in 2 mL water were added. The pH value was adjusted to 3.0-5.0 with 2.0 M NaOH. The mixturewas added with 10 mL methanol and stirred for 15 min at room temperature, and warmed at 80 C for 18 h. The solution was allowed to evaporate at room temperature. After one day, colorless acicular crystals of 2 were isolated with a yield of 125 mg (34.5%). Anal. calcd. for C11H18N2O9Ca (Mr 362.35): C, 36.4; H,5.0; N, 7.7; found: C, 36.5; H, 5.1; N, 8.0. IR (cm1): 3450sb,1633s, 1407s, 1364m, 1315w, 1119w, 920w, 887w, 710w, 621w,553w, 487w.
  • 43
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • calcium chloride [ No CAS ]
  • Ca2(H2O)6[Ca2(1,3-pdta)2(H2O)2]*4H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
43.6% With potassium hydroxide In methanol at 20 - 80℃; for 18.25h; 2.5. Synthesis of Ca2(H2O)6[(Ca2(1,3-pdta)2(H2O)2].4H2O (4) Compared with the previous report [9], preparation of 4 was improved as follow. 1,3-H4pdta (306 mg, 1.0 mmol) was dissolved in 5 mL water. A solution of CaCl2 (110 mg, 1.0 mmol) in 2 mL water was added. The pH value was adjusted to 7.0 with 2.0 M NaOH. The mixture was stirred for 15 min at room temperature, and warmed at 80 C for 18 h. The solution was allowed to evaporate at room temperature. After one week, colorless bulk crystals of 4 were isolated with a yield of 107 mg (43.6%).
  • 44
  • [ 67-56-1 ]
  • [ 1939-36-2 ]
  • [ 7732-18-5 ]
  • calcium chloride [ No CAS ]
  • K4[Ca2(1,3-propylenediaminetetraacetate)2]*2(water)*2(methanol) [ No CAS ]
YieldReaction ConditionsOperation in experiment
14.2% With potassium hydroxide at 20 - 80℃; for 18.25h; 2.4. Synthesis of K4[Ca2(1,3-pdta)2].2H2O.2CH3OH (3) 1,3-H4pdta (306 mg, 1.0 mmol) and CaCl2 (110 mg, 1.0 mmol) was dissolved in 1.0 mL water. The pH value of the mixture was adjusted to 9.0 with 2.0 M KOH. The solution was added with 10 mL methanol and stirred for 15 min at room temperature, and warmed at 80 C for 18 h. The mixture was allowed to evaporate at room temperature. After one day, colorless bulk crystals of 1 were isolated with a yield of 67 mg (14.2%). Anal. calcd. for C24H40N4O20Ca2K4 (Mr 941.16): C, 30.6; H, 4.2; N, 6.0; found: C,30.9; H, 3.7; N, 5.7. IR (cm1): 3428sb, 2961w, 2845w, 1594s,1415m, 1334w, 1288vw, 1263w, 1248w, 1171w, 1116w, 1009w,935w, 800w, 709w,621w.
  • 45
  • [ 109-76-2 ]
  • [ 79-11-8 ]
  • [ 1939-36-2 ]
YieldReaction ConditionsOperation in experiment
Stage #1: Trimethylenediamine; chloroacetic acid With sodium hydroxide; calcium oxide In water at 50 - 70℃; for 6.5h; Stage #2: With chloropropionic acid In water at 15 - 55℃; for 5h; 2.4 2.2.1. Preparation of (1,3-propanediamine-N,N,N'-triacetic-N'-3-propionic) acid, H4pd3ap (Condensation mixture) Solution A Monochloroacetic acid (11.50 g, 120 mmol) was dissolvedin 42 ml of demineralized water and 4.70 g (84 mmol) ofcalcium oxide was added to the solution. The pH rose from 1.0 to11.2. Subsequently, 3.11 g (42 mmol) of 1,3-propanediamine wasadded within 10 min. The temperature was kept at about 50 °Cwithout additional heating. After 1 h the temperature wasincreased to 70 °C and the resulting mixture was left for an additional5.5 h. During the entire reaction the pH was kept constantat 7.5-8.0 by the addition of calcium oxide. At the end of the reaction,a total of 1.90 g (34 mmol) of calcium oxide was added. Thereaction mixture was filtered warm over a glass filter to removethe excess of calcium hydroxide. The reaction mixture (volume50 ml) contains H3pd3a (50%), H4pdta (18%) and H2pdda (23%)ligands. This was checked by means of chromatography of copper(II) complexes within the above mixture. To the reaction mixturea solution of 9.44 g (236 mmol) NaOH in 15 ml of water was added.The deposited Ca(OH)2 was separated by filtration under vacuum;Solution B: A solution obtained by dissolving 4.53 g (42 mmol) of 3-chloropropionic acid in 10 ml of water was cooled in an ice bathand carefully neutralized with a cold solution of 1.68 g NaOH(42 mmol) in 5 ml of water, making sure that the solution temperaturedid not exceed 15 °C; The Solution B was then added to SolutionA (pH 7.5). The reaction mixture was gradually warmed upwith stirring to 55 °C during 5 h (where pH was maintained at8 by NaOH (1.68 g, 42 mmol in 5 ml of water). The volume ofsolution was held on 50 ml.
  • 46
  • [ 1939-36-2 ]
  • [ 401792-02-7 ]
  • 1,3-propanediamine-N,N,N′,N′-tetrakis[(2-(aminomethyl)-1,6-dimethyl-3-(phenylmethoxy)-4(1H)-pyridinone)acetamide] [ No CAS ]
YieldReaction ConditionsOperation in experiment
With benzotriazol-1-ol; dicyclohexyl-carbodiimide In N,N-dimethyl-formamide at 55℃; for 6h; Inert atmosphere; Microwave irradiation;
Stage #1: 1,3-propanediaminetetraacetatic acid With benzotriazol-1-ol; dicyclohexyl-carbodiimide In N,N-dimethyl-formamide at 20℃; for 3h; Inert atmosphere; Stage #2: 2-(aminomethyl)-1,6-dimethyl-3-(phenylmethoxy)-4(1H)-pyridinone In N,N-dimethyl-formamide at 20℃; for 144h; Inert atmosphere;
  • 47
  • [ 1939-36-2 ]
  • [ 5743-04-4 ]
  • [Cd2(1,3-propanediamine-N,N,N',N'-tetraacetate)(H2O)2]n [ No CAS ]
YieldReaction ConditionsOperation in experiment
85% With 1H-imidazole In water at 200℃; for 96h; Autoclave; High pressure; [Cd2(pdt)(H2O)2]n (1) A mixture of Cd(OAc)2*2H2O (0.4 mmol), imidazole (0.8 mmol) and 1,3-propanediamine-N,N,N',N'-tetraacetic acid (0.1 mmol) in 12 mL H2O was stirred for 15 min at room temperature (the pH value of the mixture was 6). The mixture was then transferred into a 25 mL Teflon-lined stainless-steel vessel, and heated at 200°C for four days under autogenously pressure. After the reaction mixture has slowly cooled down to room temperature, colorless block-like crystals of 1 were filtered off, washed with distilled water, and dried in air. Yield: ca. 85%. Elemental analysis for C11H18Cd2N2O10: Calc. C, 23.46; H, 3.22; N, 4.98. Found: C, 23.35; H, 3.16; N, 4.89%. IR (KBr pellet, cm-1): 3515 s, 3349 w, 3256 w, 2941 m, 2910 m, 2841 m, 2761 w, 2765 w, 2550 w, 2346 w, 2099 w, 1665 w, 1590 s, 1573 s, 1439 m, 1413 s, 1331 m, 1309 w, 1292 w, 1240 m, 1185 w, 1166 m, 1136 m, 1119 m, 1081 w, 1056 w, 1001 m, 976 m, 938 m, 916 m, 883 m, 839 w, 767 w, 729 w, 644 w, 611 w, 567 w, 531 w.
  • 48
  • [ 1939-36-2 ]
  • [ 99-31-0 ]
  • [ 6080-56-4 ]
  • [Pb4(1,3-propanediamine-N,N,N',N'-tetraacetate)(5-aminoisophthalate)2(H2O)4]n [ No CAS ]
YieldReaction ConditionsOperation in experiment
60% With 1H-imidazole In water at 200℃; for 96h; Autoclave; High pressure; [Pb4(pdt)(aip)2(H2O)4]n (2) A mixture of Pb(OAc)2*3H2O (0.6 mmol), imidazole (1.2 mmol), 5-aminoisophthalic acid (0.2 mmol) and 1,3-propanediamine-N,N,N',N'-tetraacetic acid (0.1 mmol) in 12 mL H2O was stirred for 15 min at room temperature (the pH value of the mixture was 6). The mixture was then transferred into a 25 mL Teflon-lined stainless-steel vessel, and heated at 200°C for four days under autogenously pressure. After the reaction mixture has slowly cooled down to room temperature, colorless prism-shaped crystals of 2 were filtered off, washed with distilled water, and dried in air. Yield: ca. 60%. Elemental analysis for C27H32N4O20Pb4: Calc. C, 20.77; H, 2.06; N, 3.59. Found: C, 20.68; H, 2.01; N, 3.48%. IR (KBr pellet, cm-1): 3453 s, 2922 s, 2854 m, 2353 w, 2031 w, 1634 s, 1567 s, 1465 m, 1435 w, 1405 s, 1372 s, 1323 m, 1235 w, 1158 w, 1130 m, 1111 w, 1076 w, 1053 w, 998 w, 971 w, 930 w, 910 w, 809 w, 773 m, 723 s, 663 w, 630 w, 561 w, 539 w, 520 w.
  • 49
  • copper(II) choride dihydrate [ No CAS ]
  • [ 1939-36-2 ]
  • [Cu2(1,3-propanediaminetetraacetate)2]n·nH2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
30.7% Stage #1: 1,3-propanediaminetetraacetatic acid With potassium hydroxide In water Stage #2: copper(II) choride dihydrate With hydrogenchloride; dihydrogen peroxide; potassium hydroxide In water at 20℃; for 730.5h;
  • 50
  • copper(II) choride dihydrate [ No CAS ]
  • [ 1939-36-2 ]
  • [ 1310-73-2 ]
  • Na5nOn[Cu2(HpdtaO2)2Cl]n·12.5nH2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
19.3% Stage #1: 1,3-propanediaminetetraacetatic acid; sodium hydroxide In water Stage #2: copper(II) choride dihydrate; sodium hydroxide With dihydrogen peroxide In water at 20℃; for 336h;
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