CN112679554A - Preparation of rhodium (I) acid salt [ RhL2]+A-And [ Rh ] andI(CO)2Cl]2method of complexing - Google Patents
Preparation of rhodium (I) acid salt [ RhL2]+A-And [ Rh ] andI(CO)2Cl]2method of complexing Download PDFInfo
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Abstract
The invention relates to a method for preparing rhodium (I) acid salt [ RhL2]+A‑And [ Rh ] andI(CO)2Cl]2method for preparing rhodium (I) acid salt [ RhL ]2]+A‑The step of complexing comprises: dropping a certain amount of dilute acid aqueous solution to acetylacetonatodicarbonyl rhodium (I) Rh under the protection of inert gasI(CO)2(acac) in dichloromethane, adding ligand L into the reaction solution, reacting for a certain time at a proper temperature, and stopping the reaction. Extracting, separating liquid, collecting organic phase solution containing product, rotary evaporating to remove solvent, and vacuum drying to obtain [ RhL2]+A‑. Preparation of Dicarbonylchlororhodium dimer [ RhI(CO)2Cl]2The method of the complex is to treat Rh with dilute hydrochloric acidI(CO)2(acac) highly efficient production of dicarbonylchlororhodium dimer [ Rh [ (. Rh.) ]I(CO)2Cl]2. The method has the advantages of simple and intuitive synthesis process, no introduction of new chemical reagents and impurities, low synthesis cost, no by-product, high product yield of over 93 percent and high purity (more than or equal to 99.5 percent), is economical and feasible, and is very suitable for industrial production.
Description
Technical Field
The invention relates to a method for preparing rhodium (I) acid salt [ RhL2]+A-And [ Rh ] andI(CO)2Cl]2process for the preparation of a complex, in particular a rhodium (I) acid salt [ RhL ]2]+A-And dicarbonyl chlororhodium dimer [ RhI(CO)2Cl]2A method of complex compound, belonging to the chemical field.
Background
Rhodium (I) complexes are an important class of noble metal organic compounds, are generally used for catalyzing asymmetric hydrogenation, cross-coupling, hydrosilylation and other reactions, and are widely applied to laboratory research and development and industrial production of advanced materials such as information materials, emerging drugs, polymers and the like.
With a wide range of catalyst products [ Rh (dielefin)2]BF4、[Rh(diolefin)2]OTf (dielefin ═ COD or NBD) and [ Rh (P-P)2]BF4(P-P ═ (S, S) Me-DuPhos or dppp) as an example, the synthesis method which has been widely used so far is [ Rh (diefin) Cl]2Rh (dielefin) acac or [ Rh (dielefin)2]BF4The preparation is carried out in organic solvent such as tetrahydrofuran or dichloromethane under the protection of nitrogen as rhodium source. The above-mentioned synthesis methods have various drawbacks, such as the chemical reagents used for the synthesis, e.g. AgBF4、AgSO3CF3、(C6H5)3CBF4The price is expensive, the operation steps are complicated, and the synthesis cost is high. Especially, it is difficult to remove chlorine ions (Cl) entrained in the product in the post-treatment stage-) Silver ion (Ag)+) Tritylcarbinium ion ((C)6H5)3C+) And the like, finally causing the low purity of the product and influencing the catalytic performance of the catalyst. And catalyst product [ RhI(CO)2Cl]2The preparation method usually takes carbon monoxide gas (CO) as a carbonyl source, is not beneficial to safety production and seriously harms the physical and psychological health of operators. Aiming at the practical situation of the production, the development of the [ RhL ] which has simple operation process, low production cost, no introduction of new impurities, high product purity and contribution to safe production is very necessary2]+A-And [ Rh ] andI(CO)2Cl]2a method for preparing the complex.
Disclosure of Invention
Aiming at the defects of the synthesis method in the prior art, the inventor provides a method for utilizing RhI(CO)2(acac) reaction with dilute acid HA to prepare rhodium (I) acid salt [ RhL2]+A-And dicarbonyl chlororhodium dimer [ RhI(CO)2Cl]2A method of complexing.
Preparation of rhodium (I) acid salt [ RhL ] of the invention2]+A-The method of the complex is as follows:
step 1, dripping a certain concentration of dilute acid H aqueous solution into a liquid under the protection of inert gasRhodium (I) acetylacetonate dicarbonyl (Rh)I(CO)2(acac) in a dichloromethane solution to form a reaction solution;
step 3, extracting, separating liquid, collecting an organic phase solution containing the product at room temperature, and removing the solvent by rotary evaporation;
step 4, vacuum drying to obtain [ RhL2]+A-；
Wherein the dilute acid H is tetrafluoroboric acid (HBF)4) Trifluoromethane sulfonic acid (CF)3SO3H) Perchloric acid (HClO)4) Nitric acid (HNO)3) Any one of the above.
Preferably, the concentration range of the dilute aqueous acid solution comprises:
tetrafluoroboric acid (HBF)4): 3.0-6.0 mol/L; trifluoromethanesulfonic acid (CF)3SO3H) The method comprises the following steps 4.0-11.0 mol/L; perchloric acid (HClO)4): 0.4-12.0 mol/L; nitric acid (HNO)3)：3.0～7.0mol/L。
Preferably, the ligand L comprises a dienic ligand or a bidentate phosphine ligand. The diene ligand is 1, 5-Cyclooctadiene (COD) or Norbornadiene (NBD). The bidentate phosphine ligand is any one of 1, 2-bis (diphenylphosphino) ethane (Dppe), 1, 3-bis (diphenylphosphino) propane (Dppp), (R, R) -ethylenebis [ (2-methoxyphenyl) phenylphosphine ] ((R, R) -DIPAMP), (+) -1, 2-bis [ (2S,5S) -2, 5-dimethylphosphite ] benzene ((S, S) -ME-DUPHOS).
Preferably, the inert gas is argon or nitrogen.
Preparation of dicarbonyl chlororhodium dimer [ Rh ] of the inventionI(CO)2Cl]2The method of the complex is as follows:
step 1, dripping a hydrochloric acid (HCl) aqueous solution with a certain concentration on acetylacetonatodicarbonylrhodium (I) Rh under the protection of inert gasI(CO)2(acac) in a dichloromethane solution to form a reaction solution;
step 3, extracting, separating liquid, collecting an organic phase solution containing the product at room temperature, and removing the solvent by rotary evaporation;
step 4, vacuum drying is carried out to obtain dicarbonyl chlororhodium dimer [ RhI(CO)2Cl]2。
Preferably, the concentration of the hydrochloric acid (HCl) aqueous solution is 1.0-4.0 mol/L.
Preferably, the inert gas is argon or nitrogen.
Reaction mechanism and beneficial effects of the invention
The invention is characterized in that Rh is utilizedI(CO)2(acac) reacts with dilute acid HA, easily removing neutral compound Hacac, generating transition state [ Rh (CO)2]+A-Then carrying out coordination and displacement reaction with ligand L to generate target complex [ RhL2]+A-. If dilute acid HA is hydrochloric acid, after Hacac is removed, dicarbonyl chlororhodium dimer [ Rh (CO) ]is directly generated2Cl]. One mechanism of the synthesis process is as follows:
RhI(CO)2(acac)+HA→[Rh(CO)2]+A-+Hacac
[Rh(CO)2]+A-+L→[RhL2]+A-+2CO↑
the method has the advantages of simple and visual synthesis process, no introduction of new chemical reagents and impurities, simple post-treatment, low synthesis cost and no by-product, and the product obtained by the method has the yield of over 93 percent and high purity (more than or equal to 99.5 percent), is economical and feasible and is very suitable for industrial production.
Drawings
FIG. 1 is a synthesis scheme of the process of the present invention.
Detailed Description
Example 1, [ Rh (COD)2]BF4Synthesis of (2)
Under the protection of argon, the initial reaction temperature is controlled to be 15 +/-2 ℃, 35.0mL of tetrafluoroboric acid with the concentration of 5.1mol/L is dripped into 10.0 g of RhI(CO)2(acac) IITo the methyl chloride solution, 12.7 g of COD were added in portions to the reaction flask. After the feeding is finished, the temperature is slowly increased to 25 ℃, the stirring is carried out for 1.5h at constant temperature, and the reaction is stopped. Extracting and separating the solution at room temperature, collecting the organic phase solution containing the product, removing the solvent by rotary evaporation, and drying in vacuum to obtain 15.43 g of orange red product [ Rh (COD) ]2]BF4The yield was 98.0% and the purity was 99.5%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh of 25.30% agreed with the theoretical value Rh of 25.34%; IR (cm)-1KBr pellet): v ismax 1060(BF4)、1030(BF4) 3012(COD) and 2936cm-1(COD), which conforms to the main characteristics of the target compound;1H NMR(300MHz,CDCl3)δ(ppm):4.67(s,8H,CH＝CH),7.47br(s,16H,CH2CH2) Meets the main characteristics of the target compound.
Example 2, [ Rh (dppe)2]Synthesis of OTf
Under the protection of argon, the initial reaction temperature is controlled at 10 +/-1 ℃, and 40.0 ml of trifluoromethanesulfonic acid with the concentration of 4.5mol/L is added dropwise into the reactor containing 12.0 g of RhI(CO)2And (acac) in dichloromethane, and reacting for 0.5h at constant temperature. Then 40.76 g of diphosphine ligand Dppe is dissolved in dichloromethane and slowly added dropwise into the reaction flask. After the addition, slowly heating to 50 ℃, and stirring for reaction for 3.0 h. Cooling to room temperature, extracting, separating, collecting the organic phase solution containing the product, rotary evaporating to remove the solvent, and vacuum drying to obtain 47.31 g of orange product [ Rh (dppe) ]2]OTf, 97.0% yield, 99.6% purity.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh of 9.78% was in agreement with the theoretical value Rh of 9.81%; IR (cm)-1KBr pellet): v ismax1153(OTf) and 1618cm-1(dppe) to match the main characteristics of the target compound;1H NMR(300MHz,CD2Cl2)δ(ppm):7.37～7.21(m,4H)，7.22～7.05(m，16H)，2.13～1.93(m，4H),31P(300MHz,CD2Cl2) And delta (ppm):57.40, which corresponds to the main characteristics of the target compound.
Example 3, [ Rh (NBD) ]2]BF4Synthesis of (2)
Under the protection of argon, the initial reaction temperature is controlled at 15 +/-2 ℃, and 40.0 ml of tetrafluoroboric acid with the concentration of 5.1mol/L is dripped into a container containing 12.0 g of RhI(CO)2(acac) in dichloromethane, followed by a slow addition of 42mL of NBD dropwise into the reaction flask. After the addition is finished, slowly raising the temperature to 35 ℃, reacting for 1.0 hour at constant temperature, and stopping the reaction. Cooling to room temperature, extracting, separating, collecting organic phase solution containing product, rotary evaporating to remove solvent, and vacuum drying to obtain 16.52 g of dark red product [ Rh (NBD) ]2]BF4The yield was 95.0% and the purity was 99.6%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh of 27.55% agreed with the theoretical value Rh of 27.51%; IR (cm)-1KBr pellet): v ismax.1053(BF4)、1038(BF4)、3057(NBD)、2995cm-1(NBD), which corresponds to a major feature of the target compound;1H NMR(300MHz,CDCl3)δ(ppm):4.47(d,8H,CH＝CH)，5.81(s,4H,CH)，8.43(s,4H,CH2) Meets the main characteristics of the target compound.
Example 4, [ Rh (COD)2]Synthesis of OTf
Under the protection of argon, the initial reaction temperature is controlled at 10 +/-1 ℃, and 40.0 ml of trifluoromethanesulfonic acid with the concentration of 4.5mol/L is added dropwise into the reactor containing 12.0 g of RhI(CO)2And (acac) in dichloromethane, and reacting for 0.5h at constant temperature. 15.2 g of COD were added to the reaction flask in portions. After the addition is finished, slowly raising the temperature to 35 ℃, reacting for 2.0 hours at constant temperature, and stopping the reaction. Cooling to room temperature, extracting, separating, collecting organic phase solution containing product, rotary evaporating to remove solvent, and vacuum drying to obtain 20.40 g dark red product [ Rh (COD) ]2]OTf, 93.7% yield, 99.6% purity.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh of 21.94% was consistent with the theoretical value Rh of 21.97%; IR (cm)-1KBr pellet): v ismax.1200(OTf), 3010(COD) and 2936cm-1(COD), which conforms to the main characteristics of the target compound;1H NMR(300MHz,CDCl3)δ(ppm):4.68(s,8H,CH＝CH),7.46br(s,16H,CH2CH2) Meets the main characteristics of the target compound.
Example 5, [ Rh (COD)2]ClO4Synthesis of (2)
Under the protection of argon, the reaction temperature is controlled within the range of 25 +/-2 ℃, 60.0mL of perchloric acid with the concentration of 0.6mol/L is dripped into a container containing 10.0 g of RhI(CO)2(acac) in dichloromethane, and 15.2 g of COD were added in portions to the reaction flask, a pink precipitate appeared. Stirring at constant temperature for 2.0h, and stopping reaction. Extracting, separating liquid, collecting organic phase solution containing product, rotary evaporating to remove solvent, vacuum drying to obtain 15.58 g pink product [ Rh (COD) ]2]ClO4The yield was 96% and the purity was 99.7%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh was 24.55% which was consistent with the theoretical value Rh of 24.57%; IR (cm)-1KBr pellet): v ismax.1100(ClO4)、622(ClO4) 3000(COD) and 2936cm-1(COD), which conforms to the main characteristics of the target compound;1H NMR(300MHz,CDCl3)δ(ppm):4.61(s,8H,CH＝CH),7.49br(s,16H,CH2CH2) Meets the main characteristics of the target compound.
Example 6, [ Rh (NBD) ]2]NO3Synthesis of (2)
Under the protection of argon, the initial reaction temperature is controlled within 15 +/-2 ℃, and 30.0mL of nitric acid with the concentration of 5mol/L is dropwise added into the mixture containing 10.0 g of RhI(CO)2(acac) in dichloromethane, then slowly adding 40mL of NBD dropwise into the reaction bottle, slowly raising the temperature to 25 ℃, reacting for 1.5h at constant temperature, and stopping the reaction. Extracting, separating liquid, collecting organic phase solution containing product, and rotary evaporating to remove solventDrying under vacuum to obtain 12.99 g of light red product [ Rh (NBD) ]2]NO3The yield was 96.0% and the purity was 99.6%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh of 29.45% agreed with the theoretical value Rh of 29.48%; IR (cm)-1KBr pellet): v ismax.1540(NO3)、1380(NO3)、3057(NBD)、3035(NBD)、3011cm-1(NBD), which corresponds to a major feature of the target compound;1H NMR(300MHz,CDCl3)δ(ppm):4.49(d,8H,CH＝CH),5.83(s,4H,CH)，8.45(s,4H,CH2) Meets the main characteristics of the target compound.
Example 7, [ Rh (CO) ]2Cl]2Synthesis of (2)
Under the protection of argon, the initial reaction temperature is controlled within 15 +/-2 ℃, and 30.0mL of hydrochloric acid with the concentration of 2mol/L is added dropwise to a container containing 10.0 g of RhI(CO)2And (acac) in dichloromethane solution, after the dropwise addition, raising the temperature to 35 ℃, and reacting for 1.5h at constant temperature. Cooling to room temperature, extracting, separating, collecting organic phase solution containing product, rotary evaporating to remove solvent, and vacuum drying to obtain 14.62 g of orange product [ Rh (CO ]2Cl]2The yield was 97.0% and the purity was 99.7%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh was 26.44% which agreed with the theoretical value Rh of 26.47%; IR (cm)-1KBr pellet): v ismax.2110(CO) and 2030cm-1(CO) corresponds to the main characteristic of the target compound.
Example 8, [ Rh (dppe) ]2]ClO4Synthesis of (2)
Under the protection of argon, 60.0mL of perchloric acid with the concentration of 0.6mol/L is dripped into a container containing 10.0 g of Rh at the reaction temperature of 25 +/-2 DEG CI(CO)2(acac) in dichloromethane, and 46.33 g of Dppe was added in portions to the reaction flask and reacted at constant temperature for 2.0 hours to stop the reaction. Extracting, separating liquid, collecting organic phase solution containing product, and rotary evaporating to remove solventThe mixture was dried in vacuo to give 37.37 g of a pale yellow product [ Rh (dppe) ]2]ClO4The yield was 96.5% and the purity was 99.7%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh was 10.25% which was consistent with the theoretical value Rh of 10.30%; IR (cm)-1KBr pellet): v ismax.1080(ClO4)、616(ClO4)、1620cm-1(dppe), consistent with the main characteristics of the target compound.1H NMR(300MHz,CD2Cl2)δ(ppm):7.36～7.23(m,4H)，7.22～7.06(m，16H)，2.13～1.94(m，4H),31P(300MHz,CD2Cl2) Delta (ppm):57.45, which corresponds to the main characteristic of the target compound.
Example 9, [ Rh (dppp) ]2]BF4Synthesis of (2)
Under the protection of argon, the initial reaction temperature is controlled at 15 +/-2 ℃, 35.0ml of tetrafluoroboric acid with the concentration of 5.lmol/L is dripped into the solution containing 10.0 g of RhI(CO)2(acac) in dichloromethane, followed by the addition of 50.0 g of dpp in portions to the reaction flask. After the addition is finished, slowly raising the temperature to 25 ℃ at room temperature, reacting for 1.5h at constant temperature, and stopping the reaction. Extracting, separating liquid, collecting organic phase solution containing product, rotary evaporating to remove solvent, vacuum drying to obtain 37.75 g light yellow product [ Rh (dppp) ]2]BF4The yield was 96.0% and the purity was 99.6%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh was 10.08% and the theoretical value Rh was 10.14%; IR (cm)-1KBr pellet): v ismax.1057(BF4)、1034(BF4) And 1583cm-1(dppp), which corresponds to the main characteristics of the target compound.1H NMR(300MHz,CD2Cl2)δ(ppm):7.28～7.18(m,10H)，7.17～6.98(m，30H)，2.25～2.09(m，8H),1.89-1.67(m，4H)，31P(300MHz,CD2Cl2) Delta (ppm):7.44, which corresponds to the main characteristic of the target compound.
Example 10, [ R ]h((R,R)-DIPAMP)2]NO3Synthesis of (2)
Under the protection of argon, 30.0mL of nitric acid with the concentration of 5mol/L is dripped into a container containing 10.0 g of Rh at the reaction temperature of 15 +/-2 DEG CI(CO)2(acac) in dichloromethane, then 62.21 g (R, R) -DIPAMP was slowly added into the reaction flask, and then the temperature was slowly raised to 35 ℃, and the reaction was maintained at constant temperature for 1.5h, and the reaction was stopped. Extracting, separating, collecting organic phase solution containing product, rotary evaporating to remove solvent, and vacuum drying at room temperature to obtain 41.11 g of orange product [ Rh ((R, R) -DIPAMP)2]NO3The yield was 96.8% and the purity was 99.6%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh of 9.46% agreed with the theoretical value Rh of 9.51%; IR (cm)-1KBr pellet): v ismax.1538(NO3)、1383(NO3) And 980cm-1((R, R) -DIPAMP), consistent with the main features of the target compound;1H NMR(300MHz,CDCl3) δ (ppm) 7.71 to 7.52(m,5H), 7.48 to 7.10(m,8H), 6.96 to 6.89(dd,1H), 6.87 to 6.78(t,1H), 6.57 to 6.47(t,1H), 6.12 to 6.04(t,1H), 5.50 to 5.39(t,1H), 3.75(s,3H), 3.62(s,3H), 3.10 to 2.80(m,1H), 2.48 to 2.20(m,2H), 2.08 to 1.83(m,1H), which satisfy the main characteristics of the target compound;31P(300MHz,CDCl3) Delta (ppm):84.8, 83.2, which meets the main characteristics of the target compound.
Example 11, [ Rh ((S, S) -ME-DUPHOS)2]Synthesis of OTf
Under the protection of argon, the reaction temperature is within the range of 10 +/-1 ℃, 40.0 ml of trifluoromethanesulfonic acid with the concentration of 4.5mol/L is dripped into a container containing 12.0 g of RhI(CO)2And (acac) in dichloromethane, and reacting for 0.5h at constant temperature. And adding 49.86 g of (S, S) -ME-DUPHOS into the reaction flask in batches, slowly heating to 35 ℃, reacting for 2.0h at constant temperature, and stopping the reaction. Cooling to room temperature, extracting, separating, collecting organic phase solution containing product, rotary evaporating to remove solvent, and vacuum drying to obtain 38.05 g light yellow product [ Rh ((S, S) -ME-DUPHOS)2]OTf, yield 94.6%,the purity was 99.7%.
The characteristic structural parameters of the target compound analyzed and detected in the embodiment are as follows:
the measured value Rh of 11.85% was consistent with the theoretical value Rh of 11.90%; IR (cm)-1KBr pellet): v ismax.1189(OTf) and 1050cm-1((S, S) -ME-DUPHOS), which meets the main characteristics of the target compound;1H NMR(300MHz,CDCl3) δ (ppm) 7.81 to 7.80(br m,4H), 7.65 to 7.64(br m,4H), 2.97(m,4H), 2.84 to 2.83(br m,4H), 2.52 to 2.46(br m,8H), 2.15 (adjuvant dq,4H), 1.71 (adjuvant dq,4H), 1.30 to 1.21(br m,12H), 0.99 to 0.96(m,12H), which satisfy the main characteristics of the target compound;31P(300MHz,C6D6) Delta (ppm):75.9, which corresponds to the main characteristic of the target compound.
Claims (9)
1. Preparation of rhodium (I) acid salt [ RhL2]+A-A method of complexing, comprising the steps of:
step 1, under the protection of inert gas, dripping a certain concentration of dilute acid H aqueous solution into acetylacetonatodicarbonylrhodium (I) RhI(CO)2(acac) in a dichloromethane solution to form a reaction solution;
step 2, adding a ligand L into the reaction solution, and stirring and reacting for 0.5-12.0 h at the temperature of 10-55 ℃;
step 3, extracting, separating liquid, collecting an organic phase solution containing the product at room temperature, and removing the solvent by rotary evaporation;
step 4, vacuum drying to obtain [ RhL2]+A-；
Wherein the dilute acid H is tetrafluoroboric acid (HBF)4) Trifluoromethane sulfonic acid (CF)3SO3H) Perchloric acid (HClO)4) Nitric acid (HNO)3) Any one of the above.
2. The method of claim 1, wherein the dilute aqueous acid has a concentration range comprising:
tetrafluoroboric acid (HBF)4)：3.0～6.0mol/L；
Trifluoromethanesulfonic acid (CF)3SO3H)：4.0～11.0mol/L；
Perchloric acid (HClO)4)：0.4～12.0mol/L；
Nitric acid (HNO)3)：3.0～7.0mol/L。
3. The method of claim 1, wherein:
the ligand L comprises a diene ligand or a bidentate phosphine ligand.
4. The method of claim 3, wherein:
the diene ligand is 1, 5-Cyclooctadiene (COD) or Norbornadiene (NBD).
5. The method of claim 3, wherein:
the bidentate phosphine ligand is any one of 1, 2-bis (diphenylphosphino) ethane (Dppe), 1, 3-bis (diphenylphosphino) propane (Dppp), (R, R) -ethylenebis [ (2-methoxyphenyl) phenylphosphine ] ((R, R) -DIPAMP), (+) -1, 2-bis [ (2S,5S) -2, 5-dimethylphosphite ] benzene ((S, S) -ME-DUPHOS).
6. The method according to any one of claims 1 to 5, wherein:
the inert gas is argon or nitrogen.
7. Preparation of dicarbonyl chlororhodium dimer [ RhI(CO)2Cl]2A method of complexing characterized in that:
step 1, dripping a hydrochloric acid (HCl) aqueous solution with a certain concentration on acetylacetonatodicarbonylrhodium (I) Rh under the protection of inert gasI(CO)2(acac) in a dichloromethane solution to form a reaction solution;
step 2, heating the reaction liquid to 30-50 ℃, and reacting at constant temperature for 1.0-3.0 h;
step 3, extracting, separating liquid, collecting an organic phase solution containing the product at room temperature, and removing the solvent by rotary evaporation;
step 4, vacuum drying is carried out to obtain dicarbonyl chlororhodium dimer [ RhI(CO)2Cl]2。
8. The method of claim 7, wherein:
the concentration of the hydrochloric acid (HCl) aqueous solution is 1.0-4.0 mol/L.
9. The method according to claim 7 or 8, characterized in that:
the inert gas is argon or nitrogen.
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| CN113980057B (en) * | 2021-10-26 | 2023-10-03 | 昆明贵金属研究所 | One-pot method for preparing diene rhodium (I) nitrate [ RhL ] 2 ]NO 3 Is synthesized by the method of (2) |
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