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With sodium hydroxide In methanol (NH4)2MoS4 dissolved in water, stirred, ligand dissolved in soln. of NaOH in MeOH, stirred, mixed, stirred for 30 min, kept over ice overnight; filtered, washed with cold water and EtOH;
In methanol; water aq. soln. of (NH4)2MoS4 added to soln. of tetraheptylammonium bromide inmethaonl/water; soln. stirred at room temp.; pptn.;
In ethanol; water according to Alonso G., et al., Inorg. Chim. Acta, 1998, 274, 108; soln.of (NH4)2WS4 and bromide in H2O/EtOH was stirred for 30 min; elem. anal.;
In water byproducts: NH4Br; 2 equiv. of alkylbromide in H2O was mixed with aq. soln. of W-compd. at 343 K, stirring at this temp. for 10 min; keeping overnight at room temp.;
guanidinium 9-tungstorhenate(V) trihydrate[ No CAS ]
[ 1643-19-2 ]
[ 4368-51-8 ]
tetrabutylammonium 9-tungstorhenate(VI)[ No CAS ]
tetra-n-heptylammonium 9-tungstorhenate(VII)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With Br2 In water; benzene shaking aq. W-complex with tetraheptylammonium bromide (in C6H6) for 1 min, standing org. layer for 12 h, partial evapn., Br2 addn.; MeOH addn., crystn. (refrigerator, 12-24 h), collection (filtration), washing (ether); elem. anal.; Bu4N-Re(VI) complex on addn. of Bu4NBr to part of original benzene soln. (before addn. of Br2);
[tetra-n-heptylammonium]6-[α-SiW11O39Co][ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water; toluene prepd. by cation-exchange react. of aq. soln. of corresponding K salt with toluene soln. of tetra-n-heptylammonium bromide; Co content analyzed by ICP spectrometry;
[tetra-n-heptylammonium]6-[α-SiW11O39Ni][ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water; toluene prepd. by cation-exchange react. of aq. soln. of corresponding K salt with toluene soln. of tetra-n-heptylammonium bromide; Ni content analyzed by ICP spectrometry;
[tetra-n-heptylammonium]5-[α-SiW11O39Fe][ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water; toluene prepd. by cation-exchange react. of aq. soln. of corresponding K salt with toluene soln. of tetra-n-heptylammonium bromide; Fe content analyzed by ICP spectrometry;
[tetra-n-heptylammonium]6-[α-SiW11O39Mn][ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water; toluene prepd. by cation-exchange react. of aq. soln. of corresponding K salt with toluene soln. of tetra-n-heptylammonium bromide; Mn content analyzed by ICP spectrometry;
[tetra-n-heptylammonium]6-[α-SiW11O39Cu][ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water; toluene prepd. by cation-exchange react. of aq. soln. of corresponding K salt with toluene soln. of tetra-n-heptylammonium bromide; Cu content analyzed by ICP spectrometry;
7K(1+)*PW11O39(7-)*12H2O=K7PW11O39*12H2O[ No CAS ]
[ 4368-51-8 ]
7(C7H15)4N(1+)*PW11O39(7-)=((C7H15)4N)7(PW11O39)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water; toluene soln. Hept4NBr in toluene was added to aq. soln. K7PW11O39*13H2O and stirred for 15 min; org. layer was separated and evapd., residue was dried at the pump for 1h at 50°C;
8K(1+)*SiW11O39(8-)*13H2O=K8SiW11O39*13H2O[ No CAS ]
[ 4368-51-8 ]
11(C7H15)4N(1+)*2K(1+)*SiW11O39(8-)*5Br(1-)=((C7H15)4N)8(SiW11O39)*3(C7H15)4NBr*2KBr[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
95%
In water; toluene soln. Hept4NBr in toluene was added to aq. soln. K8SiW11O39*13H2O and stirred for 30 min; org. layer was separated and evapd.; elem. anal.;
(tetraheptylammonium)7.5H6.5[NaP5W30O110][ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water to stirred aq. soln. of H14(NaP5W30O110)*25.5H2O added soln. of tetraheptylammonium bromide dropwise; stirred for 6 h; separated, purified in mixt. of H2O/MeCN;
Stage #1: copper(II) nitrate hexahydrate; K8[α-SiW11O39]*13H2O In water at 55℃; for 1.5h;
Stage #2: tetraheptylammonium bromide In water; toluene at 20℃;
Stage #1: K8[α-SiW11O39]*13H2O; iron(III) chloride hexahydrate In water at 55℃; for 1.5h;
Stage #2: tetraheptylammonium bromide In water; toluene at 20℃;
Phase transfer
A slight modification of the method introduced by Katsoulis and Pope [2] was used.Typically, an unbuffered 10 mM aqueous solution of the potassium salt of TMSPOTwas shaken briefly with an equal volume of the stoichiometric amount of THABr in toluene.The concentration of THABr solution was 50 mM for PW11Co and PW11Zn, and60 mM for SiW11Co and SiW11Zn. After the two phases had been allowed to settle for10 min, they were separated. The organic layer at this stage was determined, via coulometricKarl Fisher titration, to contain between 20 and 25 water molecules perTMSPOT. Next, the wet toluene was removed by heating to 50 °C under vacuum. Thesolid was dissolved in hexane and the hexane solution was refluxed in the presence ofan equal volume of water for 20 min at 60 °C. It took six refluxing extractions toremove all K+ and Br- ions. Next, the hexane was removed by heating at 50 °C undervacuum on a Schlenk line. Dry toluene was added using a gas tight syringe. Typically,the final water concentration was then around 5 mM. For the experiments with controlledamounts of water, wet solution containing the same ion concentration was addedusing gas tight syringes.
Phase transfer
A slight modification of the method introduced by Katsoulis and Pope [2] was used.Typically, an unbuffered 10 mM aqueous solution of the potassium salt of TMSPOTwas shaken briefly with an equal volume of the stoichiometric amount of THABr in toluene.The concentration of THABr solution was 50 mM for PW11Co and PW11Zn, and60 mM for SiW11Co and SiW11Zn. After the two phases had been allowed to settle for10 min, they were separated. The organic layer at this stage was determined, via coulometricKarl Fisher titration, to contain between 20 and 25 water molecules perTMSPOT. Next, the wet toluene was removed by heating to 50 °C under vacuum. Thesolid was dissolved in hexane and the hexane solution was refluxed in the presence ofan equal volume of water for 20 min at 60 °C. It took six refluxing extractions toremove all K+ and Br- ions. Next, the hexane was removed by heating at 50 °C undervacuum on a Schlenk line. Dry toluene was added using a gas tight syringe. Typically,the final water concentration was then around 5 mM. For the experiments with controlledamounts of water, wet solution containing the same ion concentration was addedusing gas tight syringes.
With hydrogenchloride In water; dimethyl sulfoxide for 0.333333h; Sonication;
2.4. Tetrahexylammonium, tetraheptylammonium, andtetraoctylammonium hexamolybdates
General procedure: A solution of 2.49 g sodium molybdate dihydrate (10.3 mmol) in7.5 mL water and 3 mL DMSO was acidified with 2.9 mL 6 M HCl(17.4mmol) over a 2 minute period. A solution of ~3.75mmol of the respectivetetraalkylammonium bromide in 2 mL DMSO (1 mL water and1 mL DMSO for tetrahexylammonium bromide) was then added veryslowly to this stirred solution. In some cases, heating up to 40 °C wasdone to completely dissolve the reactants. This solution was stirred for5 min before being placed under continuous sonication at 40% amplitudefor 15min and an amorphous yellow mass was collected via vacuumfiltration. In the case of the tetraoctyl- and tetraheptyl-ammoniumsalts, the solid collected were triturated and sonicated for 5 min withwater to remove any excess halide salts. Recrystallization of theresulting solidswas achieved by dissolving the crude products in heated(~80 °C) acetonitrile followed by chilling to ca. -10 °C for a period of atleast 24 h. The resulting materials were dried in a desiccator over 3 Åmolecular sieves.
3.4
(4) At room temperature, To a solution of (2S, 5R) -6- (sulfooxy) -7-oxo-1,6-diazabicyclo [3.2.1] Formamide was added 21.8 g (1.22 eq) of tetraheptylammonium bromide, After stirring for 1 h, the product was extracted with dichloromethane After drying with anhydrous sodium sulfate, Concentration gave a pale yellow oil.