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inquiry2,4-pyridinedicarboxylic acid monohydrate
Conditions | Yield |
---|---|
With KF In water High Pressure; aq. solns. 2 equiv. of N-compd., CuCl2 and 1.0 M KOH were stirred for 2 min, KF was added to adjust the Cu:OH:K ratio to 1:6:34.6, heating in a teflon-lined autoclave for 24 h at 200 °C; cooling to room temp. with 0.1 °C/min rate, crystals were filtered off, elem. anal.; | 72% |
2,4-pyridinedicarboxylic acid monohydrate
water
1,10-phenanthroline hydrate
Conditions | Yield |
---|---|
With NaOH In water High Pressure; mixt. of Cu(NO3)2*3H2O, 2,4-pyridinedicarboxylic acid monohydrate, 1,10-phenanthroline monohydrate, NaOH, H2O placed in bomb, heated at 100°C for 4 d, cooled to room temp. slowly; filtered; elem. anal.; | 71.4% |
2,4-pyridinedicarboxylic acid monohydrate
Conditions | Yield |
---|---|
With KOH; H2O2 In water addn. of V2O5 to KOH soln., stirring with heating (15 min), then cooling (0°C), addn. of 30% H2O2, stirring (5 min), filtration, dissolving ppt. with H2O2, stirring combined filtrates (5 min, pptn.), addn. ofKOH and ligand, stirring (30 min); filtration, EtOH addn. (5°C, 12 h), filtration, dissolving the ppt. in 30% H2O2, fractional crystn. on EtOH addn. and cooling to 5°C, drying (vac.); elem. anal.; | 57% |
2,4-pyridinedicarboxylic acid monohydrate
Conditions | Yield |
---|---|
With KOH; KCl In water High Pressure; 1.8 equiv. of the N-compd. neutralized with KOH and 1 equiv. of CuCl2 inH2O were stirred for 5 min, 1 equiv. of MnCl2 and KCl was added (Cu:OH: K molar ratio was 1:4:27), teflon-liend steel autoclave, 200 °C for 17 h; rapid cooling to room temp. by quenching in a water bath, crystals were filtered off in vac., elem. anal.; | 46% |
2,4-pyridinedicarboxylic acid monohydrate
cobalt(II) chloride
Conditions | Yield |
---|---|
With benzene-1,2-dicarboxylic acid; KOH In water the N-compd. and 1 equiv. of phthalic acid were deprotonated with 1.0 M KOH, 0.5 equiv. of CuCl2 soln. was added dropwise, stirring for 5 min, 1.5 equiv. of CoCl2 was added (Cu:OH ratio was 1:4.5), teflon-lined autoclave, 190 °C for 24 h; slow cooling (6 h) to room temp., crystals were filtered off, elem. anal.; | 32% |
With KOH In water the N-compd. was deprotonated with 1.0 M KOH, 0.5 equiv. of CuCl2 soln. was added dropwise, stirring for 5 min, 1.5 equiv. of CoCl2 was added (Cu:OH ratio was 1:4.5), teflon-lined autoclave, 190 °C for 24 h; | 0% |
2,4-pyridinedicarboxylic acid monohydrate
cobalt(II) chloride
Conditions | Yield |
---|---|
With KOH In water High Pressure; 2 equiv. of N-compd. and 1.0 M KOH in H2O were added to CuCl2 soln., then 3 equiv. of CoCl2 soln. was added (Cu:OH ratio was 1:7), teflon-lined stainles steel autoclave, 200 °C over 14 h; cooling to 80 °C with 0.1 °C/min rate, crystals were manually sepd. from other two products under microscope, elem. anal.; | 30% |
2,4-pyridinedicarboxylic acid monohydrate
water
zinc(II) sulfate
[Zn(2,4-pyridinedicarboxylate)(H2O)4]*H2O
Conditions | Yield |
---|---|
With NaOH In water NaOH (4 mmol) soln. was added to an aq. suspn. of a ligand (2.0 mmol); stirring for 30 min; then ZnSO4 (2 mmol) soln. was added (final pH 4.04); slow evapn. of the soln. at 298 K; elem. anal.; |
2,4-pyridinedicarboxylic acid monohydrate
water
zinc(II) sulfate
sodium hydroxide
Conditions | Yield |
---|---|
In water NaOH (2 mmol) soln. was added to an aq. suspn. of a ligand (2.0 mmol); stirring for 30 min; then ZnSO4 (1 mmol) soln. was added (final pH 4.5); slow evapn. of the soln. at 298 K; elem. anal.; |
2,4-pyridinedicarboxylic acid monohydrate
water
[Ni(H2O)6][Ni(2,4-pyridinedicarboxylate)2(H2O)2]
Conditions | Yield |
---|---|
With NaOH In water Ni-contg. compd. (2 mmol) was added to an aq. suspn. of a ligand (2.0 mmol); NaOH soln. (0.1 N) was added with stirring at 80°C; (final pH 4.21 at 298 K); slow evapn. of the soln. at 298 K; elem. anal.; |
2,4-pyridinedicarboxylic acid monohydrate
water
Conditions | Yield |
---|---|
With NaOH In sodium hydroxide; water aq. NaOH; organic ligand dissolved in H2O and NaOH; metal salts combined; added toligand soln.; react. mixt. left for several weeks at room temp.; filtered; elem. anal.; |
2,4-pyridinedicarboxylic acid monohydrate
Conditions | Yield |
---|---|
Multi-step reaction with 2 steps 1: NaOH / water; sodium hydroxide 2: neat (no solvent) View Scheme |
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