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In methanol CO bubbled through soln. of RhCl3 at 65°C for 20 h; CH3OH evapd. by passing N2 through soln., crystals sublimed (vac.);
90%
In methanol 65°C, 15 h; dissolution (hexane), crystallization (-25°C);
With water In neat (no solvent) CO passed over RhCl3*3H2O at 100°C in the presence of water (Inorg. Synth. 8 (1966) 221);
With water CO passed over RhCl3*3H2O at 100°C in presence of moisture (J.A. Mccleverty, G. Wilkinson, Inorg. Synth. 8 (1966) 221);
In not given at 100°C in the presence of moisture; Inorg. Synth. 8 (1966) 221;
With water In neat (no solvent) CO gas passed over RhCl3*3H2O powder at 100°C in the presence of water (J.A.McCleverty, G.Wilkinson, Inorg. Synth. 8, (1966), 221);
With water In neat (no solvent) CO passed over RhCl3*3H2O at 100 °C in presense moisture; J.A. McCleverty, G. Wilkinson, Inorg. synth. 8 (1966) 221.;
With H2O In neat (no solvent) CO gas passed over RhCl3*3H2O at 100°C in the presence of moisture;
In ethanol according to Powell, J. & Shaw, B. L. (1968), J. Chem. Soc. A, pp. 211-212; bubbling CO through refluxing ethanolic soln. of RhCl3*3H2O;; extraction of dry residue with boiling light petroleum;;
With H2O In neat (no solvent) passing CO over RhCl3*3H2O at 100 °C in presence of moisture; J.A. McCleverty, G. Wilkinson, Inorg. Synth. 8 (1966) 211-214.;
In ethanol addn. of ethanolic soln. of AP to a constantly stirred ethanolic soln. of RhCl3*3H2O at room temp., pptn.; filtration, washing with ethanol and ether, drying in vac. over fused CaCl2, elem. anal.;
With carbon monoxide In ethanol under argon, at 25°C, CO bubbled slowly through the solution for 4 h, CO athmosphere maintained for 12 h, filtered, washed (hexane), dissolved in chloroform; chromatographed (silica gel in hexane), eluted with CHCl3/hexane (2/1), evaporated the pale yellow band, recrystd. from CH2Cl2/n-hexane; elem. anal., NMR;
With LiCl; CO In 2-methoxy-ethanol; toluene byproducts: CO; High Pressure; Under N2, a suspn. of RhCl3*3H2O and LiCl in 2-methoxyethanol is placed under 50 psi CO at 140-145°C for 60-90 min yielding yellow {Rh(CO)2Cl2}(1-). Filtn., addn. of PNP in 2-methoxyethanol/toluene, refluxing for 40 min yields red soln.; Cooling, filtn., slow addn. of Et2O yields crystals, elem. anal.;
With hydrazinium dihydrochloride (catalyst) In ethanol; water mixt. of RhCl3*3H2O and KBr in H2O boiled (few min until red-brown soln. of RhBr6(3-) obtained), addn. of ligand in hot EtOH, immediately orange, addn. of hydrazinium dihydrochloride, refluxed (few min); filtration, filtrate kept overnight in a refrigerator, crystn., washed (ethanol, acetone, diethyl ether), evapn. (40°C); elem. anal.;
With hydrogenchloride In glycerol RhCl3*3H2O mixed with ligand, dissolved in glycerol, heated at 170°C for 24 h, cooled to room temp., HCl added; refrigerated overnight, ppt. filtered, washed with HCl and MeOH, dissolved in 3 portions of CH2Cl2, pptd. (hexanes) from first 2 portions, dried, third portion evapd., product combined; elem. anal.;
rhodium(III) 4'-methyl-2,2':6',2''-terpyridine trichloride[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
92%
In ethanol mixt. of RhCl3 and the terpyridine in abs. EtOH refluxed (2.5 h); mixt. cooled to room temp., yellow ppt. filtered, washed several times (EtOH and ether), dried (vac.);
With triphenylphosphine In ethanol addn. of a hot soln. of RhCl3*3H2O to a hot sol of PPh3 under N2, refluxing (0.5 h); hot filtn., washing of red crystals (anhyd. Et2O, under N2), drying in vac.;
Stage #1: rhodium(III) chloride trihydrate; 1,3-dioxo-4-phenyl-2H-pyrrolo<3,4-c>quinoline In ethanol; water at 90℃; for 2h; Reflux;
Stage #2: (R)-1-(pyridin-2-ylmethyl)pyrrolidine-2-carboxylic acid In ethanol; water at 90℃; for 16h; Reflux;
A mixture of 4-phenylpyrrolo[3,4-c]quinoline-1,3(2H)-dione (1a; 21.9 mg, 80.0 μmol) and RhCl3·3H2O (10.5 mg, 80.0 μmol) in EtOH/H2O 1:1 (8.0 mL) was refluxed at 90 °C for 2 h. To the resulting dark solution was added (R)-N-(pyridin-2-ylmethyl)proline (18.3 mg, 80.0 μmol) and the reaction mixture was refluxed at 90 °C for further 16 h. Then, the solvent was removed and the crude material was purified by silica gel chromatography with CH2Cl2/MeOH (gradient 50:1 to 20:1). The combined product eluents were dried in vacuo.
Stage #1: rhodium(III) chloride trihydrate; 1,3-dioxo-4-phenyl-2H-pyrrolo<3,4-c>quinoline In ethanol; water at 90℃; for 2h; Reflux;
Stage #2: (S)-1-(pyridin-2-ylmethyl)pyrrolidine-2-carboxylic acid In ethanol; water at 90℃; for 16h; Reflux;
A mixture of 4-phenylpyrrolo[3,4-c]quinoline-1,3(2H)-dione (1a; 21.9 mg, 80.0 μmol) and RhCl3·3H2O (10.5 mg, 80.0 μmol) in EtOH/H2O 1:1 (8.0 mL) was refluxed at 90 °C for 2 h. To the resulting dark solution was added (S)-N-(pyridin-2-ylmethyl)proline (18.3 mg, 80.0 μmol) and the reaction mixture was refluxed at 90 °C for further 16 h. Then, the solvent was removed and the crude material was purified by silica gel chromatography with CH2Cl2/MeOH (gradient 50:1 to 20:1). The combined product eluents were dried in vacuo
Stage #1: rhodium(III) chloride trihydrate; 2-benzyl-4-phenylpyrrolo[3,4-c]quinoline-1,3(2H)-dione In ethanol; water at 90℃; for 2h; Reflux;
Stage #2: (R)-1-(pyridin-2-ylmethyl)pyrrolidine-2-carboxylic acid In ethanol; water at 90℃; for 16h; Reflux;
A mixture of 2-benzyl-4-phenylpyrrolo[3,4-c]quinoline-1,3(2H)-dione (1b; 29.2 mg, 80.0 μmol) and RhCl3·3H2O (10.5 mg, 80.0 μmol) in EtOH/H2O 1:1 (8.0 mL) was refluxed at 90 °C for 2 h. To the resulting dark solution was added (R)-N-(pyridin-2-ylmethyl)proline (18.3 mg, 80.0 μmol) and the reaction mixture was refluxed at 90 °C for further 16 h. The solvent was removed and the crude material was purified by silica gel chromatography with CH2Cl2/MeOH (gradient 50:1 to 20:1). The combined product eluents were dried in vacuo
Stage #1: rhodium(III) chloride trihydrate; 2-benzyl-4-phenylpyrrolo[3,4-c]quinoline-1,3(2H)-dione In ethanol; water at 90℃; for 2h; Reflux;
Stage #2: (S)-1-(pyridin-2-ylmethyl)pyrrolidine-2-carboxylic acid In ethanol; water at 90℃; for 16h; Reflux;
A mixture of 2-benzyl-4-phenylpyrrolo[3,4-c]quinoline-1,3(2H)-dione (1b; 29.2 mg, 80.0 μmol) and RhCl3·3H2O (10.5 mg, 80.0 μmol) in EtOH/H2O 1:1 (8.0 mL) was refluxed at 90 °C for 2 h. To the resulting dark solution was added (S)-N-(pyridin-2-ylmethyl)proline (18.3 mg, 80.0 μmol) and the reaction mixture was refluxed at 90 °C for further 16 h. The solvent was removed and the crude material was purified by silica gel chromatography with CH2Cl2/MeOH (gradient 50:1 to 20:1). The combined product eluents were dried in vacuo
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