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cis-{(ethylenediamine)bis(1,3,9-trimethylxanthine)platinum(II)} nitrate dihydrate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In water byproducts: AgI; aq. AgNO3 and (en)PtI2 in distd. water were heated ca. 60°C with stirring for 2 h, AgI was filtered, a warm aq. soln. of 1,3,9-TMX was added to filtrate with stirring; after several ds of slow evapn. well-formed crystals were harvested;
In acetone soln. isocaffeine in acetone added dropwise to stirred soln. (Pt2Cl2(PEt3)4)(BF4)2 in acetone under N2 atm. at 25°C and stirred for 90 min; soln. evapd. under reduced pressure, Et2O slowly added, ppt. recrystd. from methanol-diethyl ether; elem. anal.;
pentaamminechlororuthenium(III) dichloride[ No CAS ]
[ 519-32-4 ]
[ 7440-66-6 ]
[ 1073148-20-5 ]
Yield
Reaction Conditions
Operation in experiment
With AgO2CCF3; HCl; air In further solvent(s) H2O acidified to pH 4 with HCl, degassed (Ar); Zn amalgam, Ru complex, AgO2CCF3, and ligand added sequentially, stirred under Ar for 30 min, airbubbled through the filtrate for 30 min; concd., pH adjusted to 2.5 with HCl, crystd. for several days at room temp. under vapor diffusion of EtOH, sepd. manually;
bis(caffeine)tetra(μ-valproato)dirhodium(II)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In ethanol Rh compd. and ligand (1:2 molar ratio) in EtOH stirred at room temp. for3 h; filtered, crystd. on storage, recrystd. (acetone), elem. anal.;
11.e e) l,3,9-Trimethyl-lH-purine-2,6(3H,9H)-dione (10)
A mixture of 5-amino-l,3-dimethyl-6-methylamino-pyrimidine-2,4(lH,3H)-dione (9) (1.5 g) and formic acid (10 mL) was refluxed for 3 h under nitrogen atmosphere. An excess of formic acid was evaporated under reduce pressure. The residue was extracted with CH2C12, washed with aq. Na2C03, dried over Na2S04 and evaporated to dryness. The residue was purified by column chromatography (eluent CH2C12 : MeOH, 10: 1) to give the title compound (0.5 g) as a white solid. NMR (400 MHz, DMSO~d6) δ (ppm): 3.22, 3.68 and 3.93 (all s, all 3H), 7.66 (s, 1 H). MS (EI) mlz: 195 |M+2]+
With N-Bromosuccinimide In acetonitrile at 20℃; for 3h;
11.f f) 8-Bromo-l,3,9-trimethyl-l /-purine-2,6(3H,9 /)-dione (11)
A mixture of l,3,9-trimethyl-lH-purine-2,6(3H,9H)-dione (10) (1.0 g, 5.15 mmol) and NBS ( 1 .2 g, 6.7 mmol) in dry MeCN (40 mL) was stirred for 3 h at room temperature. Water (30 mL) and CH2C12 (150 mL) was added, the organic phase was separated, dried over Na2S04 and evaporated to dryness. The residue was purified by column chromatography (CH2C12 : MeOH, 9: 1) to give the title compound (0.57 g) as a white solid with m.p. >200 °C. 1H NMR (400 MHz, DMSO-d6) δ (ppm): 3.22, 3.69 and 3.88 (all s, all 3H). MS (EI) mlz: 375 [M+2]+
8-(3,5-dimethyl-1H-pyrazol-1-yl)-1,3,9-trimethyl-3,4,5,9-tetrahydro-1H-purine-2,6-dione[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
85%
With ammonium peroxydisulfate; copper(I) bromide In water; acetonitrile at 80℃; for 12h; Schlenk technique; Inert atmosphere; regioselective reaction;
27%
With dichloro(dimethylglyoxime)(dimethylglyoximato)cobalt(III); 9-(2-mesityl)-10-methylacridinium perchlorate In 1,2-dichloro-ethane at 20℃; for 24h; Irradiation; Inert atmosphere; Schlenk technique; Molecular sieve; regioselective reaction;
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