Synthesis of p toluidine o sulfonic acid from p toluidine by sulfonation in solvent was studied,and effects of various reaction conditions or factors on the reaction were discussed in detail.As a result,the follow...Synthesis of p toluidine o sulfonic acid from p toluidine by sulfonation in solvent was studied,and effects of various reaction conditions or factors on the reaction were discussed in detail.As a result,the following optimum process conditions are presented:50 mL dichlorobenzene,2%~5% oleum,molar ratio of sulfonating agent to p toluidine is 1.10~1.12,oleum is dropped in the reaction system in 10 min or so,sulfate formation time is 2 h,distillation lasts 8 h.Under the above conditions,the purity and the yield of p toluidine o sulfonic acid are better than that of the same product made in Japan.展开更多
An efficient new method has been developed to synthesize N2‐alkyl 1,2,3‐triazole products by tol‐uenesulfonic acid (TsOH) catalyzed addition of N1‐Ts substituted 1,2,3‐triazoles to olefins. The reac‐tions of m...An efficient new method has been developed to synthesize N2‐alkyl 1,2,3‐triazole products by tol‐uenesulfonic acid (TsOH) catalyzed addition of N1‐Ts substituted 1,2,3‐triazoles to olefins. The reac‐tions of monosubstituted and unsubstituted triazole substrates with various olefins, including vinyl esters, are explored.展开更多
The crystal and molecular structure of diethyl l-(p-toluenesulfon-amido ) - p chlofoPhenylmet hylphosphonate has been determined by X- ray d iffractionmethod- The crystal (C18,H23,ClNO5PS) is monoclinic with space gro...The crystal and molecular structure of diethyl l-(p-toluenesulfon-amido ) - p chlofoPhenylmet hylphosphonate has been determined by X- ray d iffractionmethod- The crystal (C18,H23,ClNO5PS) is monoclinic with space group P21/c, a =8. 162(6), b= l8. O64(7), c= l4. 362(4) A, β=96. 29(3)°, V=2lO4. 7 A3, M.=431, 88, Z=4, Dx= l. 364 g/cm3, μ, = 3. 765 cm-1, F(000) = 904, R=0. 047 andRw=0. 0049 for 998 reflections with I>3σ(I). The 1H NMR spetrum of the title com-pound shows that the two ethoxy groups are magnetic nonequivalent, which is in agree-ment with its X-ray analysis result-展开更多
Sludge palm oil (SPO) is an attractive feedstock and a significant raw material for biodiesel production. The use of SPO can lower the cost ofbiodiesel production significantly. In this study biodiesel fuel was prod...Sludge palm oil (SPO) is an attractive feedstock and a significant raw material for biodiesel production. The use of SPO can lower the cost ofbiodiesel production significantly. In this study biodiesel fuel was produced from SPO by esterification process using P-toluenesulfonic acid (PTSA) as acid catalyst in different dosages in presence of methanol to convert free fatty acid (FFA) to fatty acid methyl ester (FAME). Batch esterification process of SPO was carried out to study the influence of PTSA dosage (0.25-10% wt/wt), molar ratio of methanol to SPO (6:1-20:1), temperature (40-80 ℃), reaction time (30-120 min). The effects of those parameters on the yield of crude biodiesel and conversion of FFA to FAME were monitored. The optimum condition for batch esterification process was 0.75% wt/wt, 10:1 molar ratio, 60 ℃ temperature and 60 minutes reaction time.展开更多
A novel tandem reductive amination/intermolecular nucleophilic aromatic substitution (SNAr) sequence has been established for the synthesis of amine containing pyrimidine in formation of one carbon-oxygen and one carb...A novel tandem reductive amination/intermolecular nucleophilic aromatic substitution (SNAr) sequence has been established for the synthesis of amine containing pyrimidine in formation of one carbon-oxygen and one carbon-nitrogen bonds in a one-pot fashion. Treatment of aldehyde with arylamine, 2-methanesulfonyl-4,6-dimeth-oxypyrimidine and sodium borohydride provides good overall yield. The p-toluenesulfonic acid (PTSA) can be used as activator and is generally needed in the reaction. Dioxane is the preferred reaction solvent, but reactions can also be carried out in tetrahydrofuran (THF), MeCN, toluene and dichloromethane. The procedure is carried out effectively in the presence of K2CO3. The reaction proceeds smoothly with aromatic aldehydes and arylamines possessing elec-tron-donating or-withdrawing groups. This method can be applied to the synthesis of the oilseed rape herbicide and is superior to the classical one in several aspects: cutting out several purification steps, minimizing solvent use and chemical waste, and saving time. Its advantages such as operational convenience, high-efficient synthesis, and starting material availability make it a desirable method for preparing amines with molecular diversity and biological activity.展开更多
文摘Synthesis of p toluidine o sulfonic acid from p toluidine by sulfonation in solvent was studied,and effects of various reaction conditions or factors on the reaction were discussed in detail.As a result,the following optimum process conditions are presented:50 mL dichlorobenzene,2%~5% oleum,molar ratio of sulfonating agent to p toluidine is 1.10~1.12,oleum is dropped in the reaction system in 10 min or so,sulfate formation time is 2 h,distillation lasts 8 h.Under the above conditions,the purity and the yield of p toluidine o sulfonic acid are better than that of the same product made in Japan.
基金supported by the National Natural Science Foundation of China (21272268 and 21472237)~~
文摘An efficient new method has been developed to synthesize N2‐alkyl 1,2,3‐triazole products by tol‐uenesulfonic acid (TsOH) catalyzed addition of N1‐Ts substituted 1,2,3‐triazoles to olefins. The reac‐tions of monosubstituted and unsubstituted triazole substrates with various olefins, including vinyl esters, are explored.
文摘The crystal and molecular structure of diethyl l-(p-toluenesulfon-amido ) - p chlofoPhenylmet hylphosphonate has been determined by X- ray d iffractionmethod- The crystal (C18,H23,ClNO5PS) is monoclinic with space group P21/c, a =8. 162(6), b= l8. O64(7), c= l4. 362(4) A, β=96. 29(3)°, V=2lO4. 7 A3, M.=431, 88, Z=4, Dx= l. 364 g/cm3, μ, = 3. 765 cm-1, F(000) = 904, R=0. 047 andRw=0. 0049 for 998 reflections with I>3σ(I). The 1H NMR spetrum of the title com-pound shows that the two ethoxy groups are magnetic nonequivalent, which is in agree-ment with its X-ray analysis result-
文摘Sludge palm oil (SPO) is an attractive feedstock and a significant raw material for biodiesel production. The use of SPO can lower the cost ofbiodiesel production significantly. In this study biodiesel fuel was produced from SPO by esterification process using P-toluenesulfonic acid (PTSA) as acid catalyst in different dosages in presence of methanol to convert free fatty acid (FFA) to fatty acid methyl ester (FAME). Batch esterification process of SPO was carried out to study the influence of PTSA dosage (0.25-10% wt/wt), molar ratio of methanol to SPO (6:1-20:1), temperature (40-80 ℃), reaction time (30-120 min). The effects of those parameters on the yield of crude biodiesel and conversion of FFA to FAME were monitored. The optimum condition for batch esterification process was 0.75% wt/wt, 10:1 molar ratio, 60 ℃ temperature and 60 minutes reaction time.
基金Project (Nos. Y407118 and D3080282) supported by the Natural Science Foundation of Zhejiang Province, China
文摘A novel tandem reductive amination/intermolecular nucleophilic aromatic substitution (SNAr) sequence has been established for the synthesis of amine containing pyrimidine in formation of one carbon-oxygen and one carbon-nitrogen bonds in a one-pot fashion. Treatment of aldehyde with arylamine, 2-methanesulfonyl-4,6-dimeth-oxypyrimidine and sodium borohydride provides good overall yield. The p-toluenesulfonic acid (PTSA) can be used as activator and is generally needed in the reaction. Dioxane is the preferred reaction solvent, but reactions can also be carried out in tetrahydrofuran (THF), MeCN, toluene and dichloromethane. The procedure is carried out effectively in the presence of K2CO3. The reaction proceeds smoothly with aromatic aldehydes and arylamines possessing elec-tron-donating or-withdrawing groups. This method can be applied to the synthesis of the oilseed rape herbicide and is superior to the classical one in several aspects: cutting out several purification steps, minimizing solvent use and chemical waste, and saving time. Its advantages such as operational convenience, high-efficient synthesis, and starting material availability make it a desirable method for preparing amines with molecular diversity and biological activity.