| 97% |
With aluminum oxide; dimethyl sulfoxide at 70℃; for 2.5h; |
|
| 96% |
With aluminum oxide; sodium iodate In hexane at 20℃; for 1h; |
|
| 96% |
With CsPbBr3 In dichloromethane at 20℃; for 12h; Irradiation; Green chemistry; |
|
| 95% |
With air In hexane at 30℃; for 2.5h; |
|
| 95% |
With chloro(4-1,5-cyclooctadiene)(1,3-bis(2,4,6-tris(diphenylmethyl)phenylimidazol-2-ylidene))rhodium(I) In neat (no solvent) at 20℃; |
|
| 94% |
With calcium hypochlorite; Montmorillonite K10 In hexane at 20℃; for 0.25h; |
|
| 94% |
With calcium hypochlorite; water; silica gel In hexane at 20℃; for 0.5h; |
|
| 94% |
With oxygen In water at 60℃; for 4h; |
|
| 93% |
With oxygen In water at 70℃; for 4.5h; |
General experimental procedure for oxidation of mercaptans
General procedure: Water (10 mL) and heterogeneous catalyst (0.12 g) and mercap-tan (10 mmol) were charged in a 100 mL round bottomed flask.The obtained reaction mixture was heated at 70C in the pres-ence of molecular oxygen under stirring. The reaction progresswas monitored by collecting the samples in half-an-hour inter-val, extracted with diethyl ether and analyzed by GC-MS. In orderto check the potential of developed catalytic system for sweet-ening of petroleum products, the kerosene oil was blended withn-dodecane mercaptan (300 ppm). The resulting sample was sub-jected for oxidation under optimized experimental conditions. Thesamples were withdrawn at various time periods, and unreactedmercaptan content was determined by using a potentiostat hav-ing a platinum counter electrode. For comparison, blank reactionswere also carried out by using MgAl-LDHMNP without CoPcS. |
| 93% |
With oxygen In N,N-dimethyl-formamide at 23℃; for 0.75h; Sonication; Green chemistry; |
|
| 92% |
With hydrogen bromide; dimethyl sulfoxide In chloroform at 20℃; for 6h; Inert atmosphere; Schlenk technique; |
General procedure for the synthesis of symmetrical disulfides:
General procedure: A mixture of thiols(1.0 mmol) and HX (0.2 mmol) in DMSO-CHCl3 (5 mL, 1:1, v/v) was stirred atroom temperature for respective time (Table 3). After the completion of thereaction, as monitored by TLC, the reaction mixture was diluted with 10 mL ofwater and extracted with CHCl3 (3 15 mL). The combined organic layerswere washed with brine (2 10 mL), dried over anhydrous Na2SO4, andevaporated in a rotary evaporator under reduced pressure. A reasonably pureproduct obtained was further purified by recrystallization using hexane-CHCl3mixture. The purity of the compound was confirmed by melting point andNMR measurements. |
| 89% |
With pyridine; methanesulfonyl chloride at 0℃; for 0.416667h; |
|
| 89% |
With epolactaene; sodium hydrogencarbonate In methanol; water at 20℃; for 0.5h; Inert atmosphere; |
5.3. General procedure for the formation of disulfides (Table 2)
General procedure: To a solution of 1 (10 mg, 26 μmol) and thiol (2.2 mol equiv) in degassed MeOH (1.0 mL) was added 0.5 M aqueous solution of NaHCO3 (1.0 mL) at room temperature. The mixture was stirred at room temperature under a nitrogen atmosphere until no further change in TLC was observed. The reaction was quenched by the addition of 1 M HCl aqueous solution, and the mixture was diluted with EtOAc. The layers were separated, the aqueous layer was extracted with EtOAc. The combined organic layer was washed with brine, dried (Na2SO4) and concentrated. The residue was purified by column chromatography to give the corresponding disulfide. The structures of diphenyl disulfide, 2,2'-dipyridyl disulfide, n-dihexyl disulfide and n-didodecyl disulfide were confirmed by MS analyses as well as comparison of the 1H NMR data with those of the authentic disulfides. |
| 83% |
With tributyltin methoxide; iron(III) chloride In acetonitrile for 2h; Ambient temperature; |
|
| 83% |
With 2,2'-(((diselanediylbis(2,1-phenylene))bis(azanediyl))bis(methylene))diphenol In acetonitrile at 20℃; for 7h; |
|
| 82% |
With iodine In methanol |
|
| 78% |
With sodium nitrite In water at 20℃; for 0.0333333h; |
|
| 73% |
With Fe(BTC); oxygen In acetonitrile at 70℃; for 6h; |
|
| 71% |
With manganese(II)carbonate; 3,4,5-trihydroxybenzoic acid; oxygen; sodium carbonate In water at 80℃; for 18h; Schlenk technique; Green chemistry; |
|
| 70% |
With oxygen In various solvent(s) for 1h; Ambient temperature; |
|
| 70% |
In water; N,N-dimethyl-formamide for 1h; Ambient temperature; |
|
| 68% |
With [bis(3,5-di-tert-butyl-phenolate-2-yl)-amine]triphenylantimony(V) In dichloromethane for 1.5h; Electrolysis; Inert atmosphere; |
General procedure: Antimony(V) and tin(IV) complexes I-V were synthesized by known procedures [17, 18, 21]. Commercially available 1-hexanethiol (98%, Aldrich), cyclohexanethiol (97%, Alfa Aesar), 4-methoxythiophenol (97%, Aldrich), and hexane (reagent grade) were used as received. Reagent grade dichloromethane was purified by a known procedure [22] and then dehydrated over CaH2. Electrochemical measurements were carried out on a IPC-Pro potentiostat with a Pt anode (d = 2 mm) in CH2Cl2 in the presence of 0.1 Mn-Bu4NClO4 (+99%) pre-dried in vacuum for 48 h at 50°C. A saturated silver chloride (Ag/AgCl/KCl) reference electrode with a water-tight diaphragm was used. The electrolysis of the thiol/complex mixture was carried out on a platinum anode (S = 70 mm2) in an undivided cell in dichloromethane using a PI-50.1 potentiostat and the constant potential mode. Prior to electrolysis, the solution was deaerated by purging with argon (5 min). The mediated electrosynthesis of disulfides was conducted at a more positive potential (by 0.2 V) than the oxidation potential of the mediator: 0.63-0.85 V (I-IV) and 1.20 V (V). The working concentration of the complexes was 0.001 mol/L. The thiol/complex ratio was 1 : 1 or 2 : 1. The time of electrolysisvaried from 1.5 to 3.0 h. After electrolysis, the disulfide was isolated by a stepwise procedure: the reaction mixture was concentrated; the supporting electrolyte was precipitated with hexane; sulfur compounds and the complexes were separated by column chromatography (silica gel as the adsorbent; elution with a 1 : 1 ethyl acetate-hexane mixture). The solution of the reaction products and unreacted thiols was subjected to electrochemical analysis (cyclic voltammetry (CV)). The current yields of the disulfides were estimated from the CV data. The products were identified by gas chromatography/mass spectrometry on a GCMS-QP2010 Ultra Shimadzu spectrometer with a combined flame photometric detector. Helium was used as the carrier gas; a SPB-1 SULFUR capillary column (30 m × 0.32 mm) was used, and silica gel served as the adsorbent, Tmax =320°C. The results of GC/MS analysis of sulfur compounds are summarized in Table 1. |
| 62% |
With CsF-Celite In acetonitrile Reflux; |
General procedures for the synthesis of symmetrical disulfides
General procedure: CsF-Celite (1.59 g) was stirred in 10 mL of acetonitrile, theappropriate thiol (5 mmol) was then added, and the solutionwas stirred for 5-48 h. The reaction progression was monitoredby TLC. Once the reaction was complete, the mixture wasfiltered, and the filtrate evaporated under reduced pressure.The resultant disulfide was characterized by 1H and 13C andused in thiosulfinate synthesis without further purification. |
| 60% |
With ferric hydrogen sulphate; dimethyl sulfoxide In ethanol at 20℃; for 3h; |
|
|
With (OHCH2CH2S)2 |
|
|
With sodium hypoiodite |
|
|
With bromine Ambient temperature; Yield given; |
|
|
With manganese(IV) oxide; molecular sieve In hexane for 1h; Heating; Yield given; |
|
|
With pyridine In methanol at 20℃; for 7h; Irradiation; reflux for 5 h; |
|
|
With chlorine dioxide In tetrachloromethane at 40℃; |
|
|
Multi-step reaction with 2 steps
1.1: NaH / tetrahydrofuran / 2 h / Heating
1.2: 99 percent / tetrahydrofuran / 48 h / Heating
2.1: 16 percent / conc. H2SO4 / toluene / 384 h / Heating |
|
|
Multi-step reaction with 2 steps
1.1: NaH / tetrahydrofuran / 2 h / Heating
1.2: 99 percent / tetrahydrofuran / 48 h / Heating
2.1: PPA / xylene / 48 h |
|
|
With oxygen In ethanol at 70℃; for 29h; |
|
|
With boron nitride; oxygen In ethanol at 70℃; for 48h; |
|
|
With tert.-butylhydroperoxide |
|
|
With C222H156Fe4N24(8+)*8C2F6NO4S2(1-) In [D3]acetonitrile at 50℃; for 11.5h; Sealed tube; |
|
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