* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
The 3000Kg-nitro ethylbenzene, 150g cobalt stearate into the oxidation reactor, was evacuated and replaced with oxygen, to the oxidation reactor through the oxygen control oxygen pressure 0.8Mpa, open stirred reactor, open the oxidation reactor steam the reaction was terminated heating, when the oxidation reaction Tanei Da to 165 , after the reaction started off steam, exhaust steam, open the cooling water, a slow cooling to 140 , 140 thermal control for 18 hours, when the amount of ketone containing up to 80percent when with the kettle and pressure oil to oxidation reaction to acid tank, acid tank to start stirring slowly added 30percent sodium hydroxide solution 100Kg, adjusted PH to 7, then add a saturated solution of sodium carbonate 30Kg, adjusted PH to 8.5, stirred for 30 minutes, allowed to stand for 1.5 hours to stop stirring, layered sodium nitrobenzene solution put to the reservoir, between nitrobenzoic acid to be recovered, the oxidation reaction of oil to the crystallization reactor, cooling to freeze 10 , centrifugal rejection filter , washing, drying in 2350kg (Melting point 78.5 ), distilled liquor recovered 495kg (including the amount of 19.16percent ketone, and then for the oxidation), inter-nitroacetophenone product yield 85.85percent.
60%
With copper; Selectfluor In water; acetonitrile at 20℃; for 4 h;
m-Nitroethylbenzene 0.2 mmol,Copper powder 0.02 mmolAnd Selectfluor 0.02mmol in turn into a 10mL pressure sealed container,Add 2 mL of a mixture of acetonitrile and water (CH3CN/H2O = 400:1).The mixture was stirred at room temperature and the reaction was monitored by TLC. The reaction was completed after 4 hours.The reaction solution was diluted with dichloromethane 10 mL,Filtered to obtain a clear solution, after distillation of the solvent, column chromatography(eluent ratio: petroleum ether to ethyl acetate volume ratio 20:1) separation,The washings were collected and the solvent was evaporated to give m-nitroacetophenone in a yield of 60percent.
Reference：
[1] Patent: CN105461565, 2016, A, . Location in patent: Paragraph 0045; 0046
[2] Patent: CN105085205, 2018, B, . Location in patent: Paragraph 0077; 0078; 0079
[3] Zhurnal Prikladnoi Khimii (Sankt-Peterburg, Russian Federation), 1959, vol. 32, p. 1806,1810; engl. Ausg. S. 1845, 1848
2
[ 586-39-0 ]
[ 7369-50-8 ]
[ 587-02-0 ]
Yield
Reaction Conditions
Operation in experiment
75%
With hydrogen In ethanol at 20℃; for 3 h;
General procedure: In a typical reaction, 0.015 g of catalyst and 2 mmol of the reactant were taken in 10 mL of ethanol under hydrogen atmosphere. The reaction was monitored by thin-layer chromatography (TLC). After complete disappearance of the starting material, the catalyst was separated by simple filtration and the solvent was removed under reduced pressure to obtain the pure product.
Reference：
[1] Advanced Synthesis and Catalysis, 2012, vol. 354, # 4, p. 663 - 669
[2] Journal of Molecular Catalysis A: Chemical, 2012, vol. 365, p. 115 - 119
[3] ChemCatChem, 2015, vol. 7, # 4, p. 635 - 642
[4] Angewandte Chemie - International Edition, 2015, vol. 54, # 9, p. 2661 - 2664[5] Angew. Chem., 2015, vol. 127, # 9, p. 2699 - 2702,3
[6] Chemical Communications, 2017, vol. 53, # 23, p. 3377 - 3380
[7] Journal of the American Chemical Society, 2018, vol. 140, # 11, p. 3940 - 3951
[8] Journal of Catalysis, 2018, vol. 364, p. 297 - 307
3
[ 586-39-0 ]
[ 7369-50-8 ]
Reference：
[1] Advanced Synthesis and Catalysis, 2012, vol. 354, # 14-15, p. 2689 - 2694
[2] Angewandte Chemie - International Edition, 2013, vol. 52, # 39, p. 10241 - 10244[3] Angew. Chem., 2013, p. 10431 - 10434
[4] Chemistry - A European Journal, 2015, vol. 21, # 11, p. 4368 - 4376
[5] Chemistry - A European Journal, 2016, vol. 22, # 5, p. 1577 - 1581
[6] Tetrahedron Letters, 1987, vol. 28, # 12, p. 1321 - 1322
[7] Journal of Organic Chemistry, 2000, vol. 65, # 26, p. 8933 - 8939
[8] Journal of Organic Chemistry, 2009, vol. 74, # 8, p. 3186 - 3188
[9] Advanced Synthesis and Catalysis, 2009, vol. 351, # 14-15, p. 2271 - 2276
[10] Journal of Catalysis, 2011, vol. 284, # 2, p. 176 - 183
[11] Organic Letters, 2013, vol. 15, # 3, p. 710 - 713
[12] Chemical Communications, 2013, vol. 49, # 23, p. 2359 - 2361
[13] ChemCatChem, 2014, vol. 6, # 11, p. 3153 - 3159
[14] Journal of the American Chemical Society, 2015, vol. 137, # 16, p. 5582 - 5589
[15] RSC Advances, 2017, vol. 7, # 6, p. 3398 - 3407
[16] Journal of Catalysis, 2018, vol. 364, p. 297 - 307
[17] Journal of the American Chemical Society, 2018, vol. 140, # 48, p. 16460 - 16463
4
[ 586-39-0 ]
[ 7369-50-8 ]
[ 15411-43-5 ]
Reference：
[1] Catalysis Today, 2013, vol. 213, p. 93 - 100
[2] Green Chemistry, 2016, vol. 18, # 5, p. 1332 - 1338
5
[ 586-39-0 ]
[ 241147-96-6 ]
[ 98-54-4 ]
[ 7369-50-8 ]
Reference：
[1] European Journal of Organic Chemistry, 2015, vol. 2015, # 33, p. 7253 - 7257
6
[ 586-39-0 ]
[ 7369-50-8 ]
[ 15411-43-5 ]
[ 587-02-0 ]
Reference：
[1] Journal of the American Chemical Society, 2008, vol. 130, # 27, p. 8748 - 8753
[2] Journal of the American Chemical Society, 2008, vol. 130, # 27, p. 8748 - 8753
[3] Advanced Synthesis and Catalysis, 2011, vol. 353, # 8, p. 1260 - 1264
[4] Journal of Molecular Catalysis A: Chemical, 2014, vol. 393, p. 257 - 262
[5] Journal of Molecular Catalysis A: Chemical, 2014, vol. 393, p. 257 - 262
[6] Journal of Molecular Catalysis A: Chemical, 2014, vol. 393, p. 257 - 262
[7] Journal of Molecular Catalysis A: Chemical, 2014, vol. 393, p. 257 - 262
[8] Journal of Molecular Catalysis A: Chemical, 2014, vol. 393, p. 257 - 262
[9] Catalysis Communications, 2015, vol. 61, p. 11 - 15
[10] Green Chemistry, 2016, vol. 18, # 5, p. 1332 - 1338
[11] Chemical Communications, 2017, vol. 53, # 12, p. 1969 - 1972
[12] Chemical Communications, 2017, vol. 53, # 23, p. 3377 - 3380
[13] Chemical Communications, 2017, vol. 53, # 23, p. 3377 - 3380
[14] Journal of the American Chemical Society, 2018, vol. 140, # 11, p. 3940 - 3951
7
[ 100-41-4 ]
[ 100-12-9 ]
[ 612-22-6 ]
[ 7369-50-8 ]
Reference：
[1] Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1988, vol. 37, # 3, p. 612 - 614[2] Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1988, # 3, p. 714 - 716
[3] Bulletin of the Academy of Sciences of the USSR, Division of Chemical Science (English Translation), 1988, vol. 37, # 3, p. 612 - 614[4] Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, 1988, # 3, p. 714 - 716
[5] Tetrahedron Letters, 1989, vol. 30, # 39, p. 5333 - 5336
[6] Journal of Organic Chemistry, 1981, vol. 46, # 13, p. 2706 - 2709
[7] Tetrahedron, 1989, vol. 45, # 9, p. 2719 - 2730
[8] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1993, # 14, p. 1591 - 1598
[9] Russian Journal of Organic Chemistry, 1993, vol. 29, # 3.2, p. 457 - 466[10] Zhurnal Organicheskoi Khimii, 1993, vol. 29, # 3, p. 546 - 558
[11] Tetrahedron, 1989, vol. 45, # 9, p. 2719 - 2730
[12] Russian Journal of Organic Chemistry, 1993, vol. 29, # 3.2, p. 457 - 466[13] Zhurnal Organicheskoi Khimii, 1993, vol. 29, # 3, p. 546 - 558
[14] Journal of Organic Chemistry, 1981, vol. 46, # 17, p. 3533 - 3537
[15] Journal of the Chemical Society, Perkin Transactions 2: Physical Organic Chemistry (1972-1999), 1982, p. 965 - 970
[16] Journal of Organic Chemistry USSR (English Translation), 1985, vol. 21, # 11, p. 2179 - 2186[17] Zhurnal Organicheskoi Khimii, 1985, vol. 21, # 11, p. 2382 - 2390
[18] Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1993, # 14, p. 1591 - 1598
[19] J. Gen. Chem. USSR (Engl. Transl.), 1987, vol. 57, p. 2280 - 2283[20] Zhurnal Obshchei Khimii, 1987, vol. 57, # 11, p. 2562 - 2565
[21] Russian Journal of General Chemistry, 1997, vol. 67, # 10, p. 1618 - 1623
[22] Russian Journal of Organic Chemistry, 1993, vol. 29, # 3.2, p. 457 - 466[23] Zhurnal Organicheskoi Khimii, 1993, vol. 29, # 3, p. 546 - 558
[24] Journal of Organic Chemistry, 1998, vol. 63, # 23, p. 8448 - 8454
[25] Synthetic Communications, 1999, vol. 29, # 12, p. 2169 - 2174
[26] Russian Journal of General Chemistry, 2000, vol. 70, # 9, p. 1413 - 1418
[27] Catalysis Communications, 2014, vol. 49, p. 82 - 86
[28] ChemPlusChem, 2013, vol. 78, # 4, p. 310 - 317
[29] Green Chemistry, 2015, vol. 17, # 6, p. 3446 - 3451
[30] Asian Journal of Chemistry, 2016, vol. 28, # 3, p. 513 - 516
Reference：
[1] Bulletin de la Societe Chimique de France, 1894, vol. <3> 11, p. 210[2] Comptes Rendus Hebdomadaires des Seances de l'Academie des Sciences, 1894, vol. 118, p. 424
[3] Journal of Medicinal Chemistry, 1968, vol. 11, p. 580 - 582
13
[ 3663-33-0 ]
[ 7369-50-8 ]
Reference：
[1] Journal of Medicinal Chemistry, 1968, vol. 11, p. 580 - 582
14
[ 3663-34-1 ]
[ 7369-50-8 ]
Reference：
[1] Journal of Medicinal Chemistry, 1968, vol. 11, p. 580 - 582
15
[ 587-02-0 ]
[ 7369-50-8 ]
Reference：
[1] Zhurnal Obshchei Khimii, 1957, vol. 27, p. 3204,3207; engl. Ausg. S. 3240, 3243
16
[ 64-17-5 ]
[ 98-95-3 ]
[ 100-12-9 ]
[ 612-22-6 ]
[ 7369-50-8 ]
[ 1701-51-5 ]
[ 10482-00-5 ]
[ 103095-31-4 ]
Reference：
[1] Journal of Organic Chemistry, 1990, vol. 55, # 12, p. 3961 - 3962
17
[ 598-58-3 ]
[ 100-41-4 ]
[ 100-12-9 ]
[ 612-22-6 ]
[ 7369-50-8 ]
Reference：
[1] Journal of the American Chemical Society, 1987, vol. 109, # 17, p. 5092 - 5097
With 1 wt.%Ir/ZrO2; hydrogen; In ethanol; at 24.84℃; under 15001.5 Torr;Autoclave;Kinetics;
General procedure: Catalytic evaluation was carried out in liquid phase in a Parrstainless steel batch reactor at 298 K using 50.0 mg of catalyst and0.1 mol L-1 of the model molecule (nitrobenzene) and the otherssubstrates, under 20 bar hydrogen pressure. All the components(catalyst, solvent and substrate) were fed to the reactor and stirredat 700 rpm. Liquid samples were taken periodically from thereactor and analyzed in a GC-MS Shimadzu GCMS-QP5050 witha capillary column -Dex 225 (Supelco). The compounds are:m-chloronitrobenzene, m-nitrotoluene, m-nitrobenzaldehyde,m-nitrostyrene, m-nitrobenzonitrile, m-nitroanisole and mdinitrobenzeneand the effect on the activity and selectivityin function of the effects conferred by the substituents wasstudied
With cobalt(II) stearate; sodium carbonate; sodium hydroxide; at 140 - 165℃; under 6000.6 Torr; for 20.0h;pH 7 - 8.5;
The 3000Kg-nitro ethylbenzene, 150g cobalt stearate into the oxidation reactor, was evacuated and replaced with oxygen, to the oxidation reactor through the oxygen control oxygen pressure 0.8Mpa, open stirred reactor, open the oxidation reactor steam the reaction was terminated heating, when the oxidation reaction Tanei Da to 165 , after the reaction started off steam, exhaust steam, open the cooling water, a slow cooling to 140 , 140 thermal control for 18 hours, when the amount of ketone containing up to 80% when with the kettle and pressure oil to oxidation reaction to acid tank, acid tank to start stirring slowly added 30% sodium hydroxide solution 100Kg, adjusted PH to 7, then add a saturated solution of sodium carbonate 30Kg, adjusted PH to 8.5, stirred for 30 minutes, allowed to stand for 1.5 hours to stop stirring, layered sodium nitrobenzene solution put to the reservoir, between nitrobenzoic acid to be recovered, the oxidation reaction of oil to the crystallization reactor, cooling to freeze 10 , centrifugal rejection filter , washing, drying in 2350kg (Melting point 78.5 ), distilled liquor recovered 495kg (including the amount of 19.16% ketone, and then for the oxidation), inter-nitroacetophenone product yield 85.85%.
60%
With copper; Selectfluor; In water; acetonitrile; at 20℃; for 4.0h;
m-Nitroethylbenzene 0.2 mmol,Copper powder 0.02 mmolAnd Selectfluor 0.02mmol in turn into a 10mL pressure sealed container,Add 2 mL of a mixture of acetonitrile and water (CH3CN/H2O = 400:1).The mixture was stirred at room temperature and the reaction was monitored by TLC. The reaction was completed after 4 hours.The reaction solution was diluted with dichloromethane 10 mL,Filtered to obtain a clear solution, after distillation of the solvent, column chromatography(eluent ratio: petroleum ether to ethyl acetate volume ratio 20:1) separation,The washings were collected and the solvent was evaporated to give m-nitroacetophenone in a yield of 60%.
With dinitrogen pentoxide; In dichloromethane; at 30℃; for 0.0133333h;Flow reactor;
General procedure: We used a interdigital triangular-single channel-pillar microglass reactor in reactions (V = 1.326 mL; mixed zone dimensions: height 150 mum, width 50 mum, reaction channel dimensions: depth 0.5 mm, width 4.5 mm, length 800 mm; heat exchange area 3600 mm2). As shown in Fig. 2, a sketch of aromatics nitration process-flow diagram controlled by microfluidic chip. The whole system consists of reactants, pumps, microreactor, thermostatic water bath and separating unit. The solvent was first added in ionic liquids and heated at 30 C in vacuum thus achieving fully mixing. Then a certain amount of N2O5 was added in the mixture. Reactants and nitrating reagents flow into the microchip and reaction channel controlled by constant pressure pump, reaction temperature adjusts by thermostatic water bath (Fig. 3). The organic phase was washed with a few portions of saturated NaHCO3 solution, then several times with water, dried with MgSO4 and the sample of the organic layer was analyzed by gas chromatography (GC) using the internal standard method. The aqueous phase was composed of nitric acid of remaining and ionic liquid which could be readily recycled by simple evaporation.
With hydrogen; In methanol; water; at 79.84℃; under 37503.8 Torr; for 12.0h;
Unless specified otherwise, all hydrogenation reactions were carried out at 353 K in small glass vials placed inside a 200-mL autoclave with vigorous magnetic stirring (P900 RPM). Conversions and selectivities were measured by 1H NMR and gas chromatographic techniques. All hydrogenated products were initially identified by using authentic commercial samples of the expected products. The recycling experiments with 1 and 2 were carried out at 353 K under 50 and 40 bar H2 pressure, respectively, with a substrate-to-Ru molar ratio of 283 and 625 in 5 mL of methanol and water, respectively. Recycling experiments with 2 covering five successive batches were also carried out with styrene as the substrate, with a styrene-to-Ru molar ratio of 625 in 5 mL of methanol. Catalyst 1 was filtered off, washed several times with methanol, and used for the second batch. For the reaction with 2, the product was separated from the aqueous solution by ethyl acetate extraction(2 x 10 mL). The aqueous solution of 2 was then reused. A few recycling experiments were also carried out, where 2 was precipitated from the water solution by the addition of acetone and reused. The results obtained by both these methods of catalyst recovery were comparable.
With hydrogen; In toluene; at 100℃; under 15001.5 - 30003 Torr; for 0.08333330000000001h;Autoclave;
The catalytic performance of Pt catalysts on raw and surfacemodifiedcarbon supports were tested for the selective hydrogenationof 3nitrostyrene using a 50 mL stainless steel autoclave withan inner Teflon coating. For a typical catalytic reaction, 0.5 mmol3-nitrostyrene and 10-40 mg catalyst were mixed in 5 mL toluene.The reactor was purged with 2 MPa H2 three times and it wassealed. The reaction was conducted at 4 MPa H2 at 100 C. The productswere analyzed by gas chromatography (Shimadzu, 2010)equipped with a capillary column (Restek-5 30 m x 0.25 mm x 0.25 mum) and a flame ionization detector (FID). Conversion wasdetermined by dividing the amount of NS consumed by the initialamount of NS; product selectivity was calculated by dividing theamount of a certain product by the amount of NS consumed.Site-time-yield was calculated by dividing the amount a certainproduct by the amount of exposed Pt atoms and reaction time.
With water; hydrazine; at 100℃; for 0.166667h;Inert atmosphere;
General procedure: The catalytic performance of several carbon materials prepared was tested in liquid-phase reduction of nitrobenzene, styrene, and 3-nitrostyrene by hydrazine. The Teflon-coated reactor was loaded with carbon catalyst, substrate, and hydrazine hydrate, purged by 0.2 MPa N2, and heated to a reaction temperature of 100 C on a heating place. The reaction mixture was stirred by a magnetic stirrer at 100 C for a certain period of time. The multiphase reaction mixture was so mixed at a stirring rate of >400 rpm that the influence of agitation was negligible. Then, the reactor was cooled by ice water and the liquid phase was separated by filtration. The liquid mixture was analyzed by gas chromatography (GL Science 390B) using decane as an internal standard. The conversion was determined from the amounts of substrate before and after reaction and the selectivity from the amount of a product divided by the total amount of all products detected.
With pyrographite; hydrazine; at 100℃; for 2h;Inert atmosphere;
General procedure: The catalytic performance of several carbon materials prepared was tested in liquid-phase reduction of nitrobenzene, styrene, and 3-nitrostyrene by hydrazine. The Teflon-coated reactor was loaded with carbon catalyst, substrate, and hydrazine hydrate, purged by 0.2 MPa N2, and heated to a reaction temperature of 100 C on a heating place. The reaction mixture was stirred by a magnetic stirrer at 100 C for a certain period of time. The multiphase reaction mixture was so mixed at a stirring rate of >400 rpm that the influence of agitation was negligible. Then, the reactor was cooled by ice water and the liquid phase was separated by filtration. The liquid mixture was analyzed by gas chromatography (GL Science 390B) using decane as an internal standard. The conversion was determined from the amounts of substrate before and after reaction and the selectivity from the amount of a product divided by the total amount of all products detected.
With hydrazine; at 100℃; for 2h;Inert atmosphere;
General procedure: The catalytic performance of several carbon materials prepared was tested in liquid-phase reduction of nitrobenzene, styrene, and 3-nitrostyrene by hydrazine. The Teflon-coated reactor was loaded with carbon catalyst, substrate, and hydrazine hydrate, purged by 0.2 MPa N2, and heated to a reaction temperature of 100 C on a heating place. The reaction mixture was stirred by a magnetic stirrer at 100 C for a certain period of time. The multiphase reaction mixture was so mixed at a stirring rate of >400 rpm that the influence of agitation was negligible. Then, the reactor was cooled by ice water and the liquid phase was separated by filtration. The liquid mixture was analyzed by gas chromatography (GL Science 390B) using decane as an internal standard. The conversion was determined from the amounts of substrate before and after reaction and the selectivity from the amount of a product divided by the total amount of all products detected.
With hydrazine; at 100℃; for 0.166667h;Inert atmosphere;
General procedure: The catalytic performance of several carbon materials prepared was tested in liquid-phase reduction of nitrobenzene, styrene, and 3-nitrostyrene by hydrazine. The Teflon-coated reactor was loaded with carbon catalyst, substrate, and hydrazine hydrate, purged by 0.2 MPa N2, and heated to a reaction temperature of 100 C on a heating place. The reaction mixture was stirred by a magnetic stirrer at 100 C for a certain period of time. The multiphase reaction mixture was so mixed at a stirring rate of >400 rpm that the influence of agitation was negligible. Then, the reactor was cooled by ice water and the liquid phase was separated by filtration. The liquid mixture was analyzed by gas chromatography (GL Science 390B) using decane as an internal standard. The conversion was determined from the amounts of substrate before and after reaction and the selectivity from the amount of a product divided by the total amount of all products detected.
With hydrazine; at 100℃; for 2h;Inert atmosphere;
General procedure: The catalytic performance of several carbon materials prepared was tested in liquid-phase reduction of nitrobenzene, styrene, and 3-nitrostyrene by hydrazine. The Teflon-coated reactor was loaded with carbon catalyst, substrate, and hydrazine hydrate, purged by 0.2 MPa N2, and heated to a reaction temperature of 100 C on a heating place. The reaction mixture was stirred by a magnetic stirrer at 100 C for a certain period of time. The multiphase reaction mixture was so mixed at a stirring rate of >400 rpm that the influence of agitation was negligible. Then, the reactor was cooled by ice water and the liquid phase was separated by filtration. The liquid mixture was analyzed by gas chromatography (GL Science 390B) using decane as an internal standard. The conversion was determined from the amounts of substrate before and after reaction and the selectivity from the amount of a product divided by the total amount of all products detected.
With hydrogen; at 49.84℃; under 30003 Torr;Catalytic behavior;
Prior to the catalytic tests, the catalysts were reduced under H2 flow (50cm3/min) at the desired reduction temperature (200 or 500C) for 3h. The hydrogenation of NS was carried out in a 50cm3 autoclave. The reactor was loaded with approximately 10mg of catalyst and 0.5cm3 of nitrostyrene (3.6mmol), purged with hydrogen to remove the air for three times. The reaction was carried out isothermally at 323K at 4MPa of H2 with a high-pressure liquid pump. Prior to the experiments the reaction mixture was stirred with a magnetic stirrer. After the reaction, the reactor was cooled below room temperature by ice-water and carefully depressurized. The obtained-products were then analyzed by a gas chromatograph attached with a flame ionization detector using decane as an internal standard.
With hydrogen; In ethanol; at 20.0℃; under 760.051 Torr; for 3h;
General procedure: In a typical reaction, 0.015 g of catalyst and 2 mmol of the reactant were taken in 10 mL of ethanol under hydrogen atmosphere. The reaction was monitored by thin-layer chromatography (TLC). After complete disappearance of the starting material, the catalyst was separated by simple filtration and the solvent was removed under reduced pressure to obtain the pure product.
With hydrogen; In toluene; at 100.0℃; under 15001.5 - 30003 Torr; for 0.0833333h;Autoclave;
The catalytic performance of Pt catalysts on raw and surfacemodifiedcarbon supports were tested for the selective hydrogenationof 3nitrostyrene using a 50 mL stainless steel autoclave withan inner Teflon coating. For a typical catalytic reaction, 0.5 mmol<strong>[586-39-0]3-nitrostyrene</strong> and 10-40 mg catalyst were mixed in 5 mL toluene.The reactor was purged with 2 MPa H2 three times and it wassealed. The reaction was conducted at 4 MPa H2 at 100 C. The productswere analyzed by gas chromatography (Shimadzu, 2010)equipped with a capillary column (Restek-5 30 m x 0.25 mm x 0.25 mum) and a flame ionization detector (FID). Conversion wasdetermined by dividing the amount of NS consumed by the initialamount of NS; product selectivity was calculated by dividing theamount of a certain product by the amount of NS consumed.Site-time-yield was calculated by dividing the amount a certainproduct by the amount of exposed Pt atoms and reaction time.
With 1 wt.%Ir/ZrO2; hydrogen; In ethanol; at 24.84℃; under 15001.5 Torr;Autoclave;Kinetics;
General procedure: Catalytic evaluation was carried out in liquid phase in a Parrstainless steel batch reactor at 298 K using 50.0 mg of catalyst and0.1 mol L-1 of the model molecule (nitrobenzene) and the otherssubstrates, under 20 bar hydrogen pressure. All the components(catalyst, solvent and substrate) were fed to the reactor and stirredat 700 rpm. Liquid samples were taken periodically from thereactor and analyzed in a GC-MS Shimadzu GCMS-QP5050 witha capillary column -Dex 225 (Supelco). The compounds are:m-chloronitrobenzene, m-nitrotoluene, m-nitrobenzaldehyde,m-nitrostyrene, m-nitrobenzonitrile, m-nitroanisole and mdinitrobenzeneand the effect on the activity and selectivityin function of the effects conferred by the substituents wasstudied
With sodium tetrahydroborate; In dimethyl sulfoxide; at 20℃; for 1.5h;
5.8 g of the crude 1-(1-iodoethyl)-3-nitrobenzene obtained in step (2),Dissolved in 50mL DMSO, sodium borohydride (1.44g, 40mmol, 2.0eq) was added in portions. The reaction was completed at room temperature for 1.5 hours after the addition, and the reaction was followed by TLC.300 mL of water was added to the reaction system, and extracted three times with ethyl acetate (100 ml * 3).The organic phases were combined and washed three times with saturated brine (50 mL * 3).The organic phase was dried over anhydrous sodium sulfate and concentrated to obtain a crude product.Distillation under reduced pressure gave 2.7 g of pure 1-ethyl-3-nitrobenzene with a yield of 90%.
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