| 95% |
With urea hydrogen peroxide adduct In ethanol at 20℃; for 0.6h; |
Typical procedure for the synthesis of disulfides catalyzed by Co(at)MCM-41 or Fe(at)MCM-41: as a typical procedure
General procedure: A mixture of thiols (1 mmol), UHP (5 mmol), and Co orFeMCM-41 (20 mg) was stirred at room temperature inethanol and the progress of the reaction was monitored by TLC.After completion of the reaction, the catalyst was removed andthe products were extracted with CH2Cl2 (3 × 10 mL). Theresults are shown in Table 7. |
| 95% |
With urea hydrogen peroxide adduct In ethanol at 20℃; for 0.4h; |
General procedure for oxidative coupling of thiols to disulfides with UHP catalyzed by Cr-MCM-41 and Mn-MCM-41
General procedure: Thiols ((1 mmol), 5 mmol UHP, and 4 mL acetone as solvent along with 25 mg catalyst were added to a 10-mL two-necked flask equipped with a stirrer. The progress of the reaction was monitored by TLC. After completion of the reaction, the catalyst was removed and the pure products were extracted with CH2Cl2(3 9 10 mL). The results are presented in Table 6. |
| 94% |
With sodium periodate In water at 20℃; for 0.0333333h; |
|
| 94% |
With urea hydrogen peroxide adduct In acetonitrile at 20℃; for 0.35h; |
|
| 93% |
With dihydrogen peroxide In acetonitrile at 20℃; for 0.666667h; Green chemistry; |
|
| 92% |
With [Mn(III)(BHBPDI)Cl]; oxygen In ethanol at 20℃; for 4h; |
|
| 92% |
With dihydrogen peroxide In ethanol at 20℃; for 0.75h; Green chemistry; |
General procedure for the oxidative coupling of thiols to the disulfides
General procedure: A mixture of thiol (1 mmol), hydrogen peroxide (0.5 mL) and the catalyst (0.005 g) in ethanol (2 mL) was stirred at ambient temperature. Reaction progress was monitored by TLC (acetone: n-hexane, 2:8). After completion of the reaction, catalyst was separated by an external magnet and washed with ethyl acetate; next, the product was extracted with ethyl acetate (5 mL 9 4). The organic layer was dried over anhydrous Na2SO4 (1.5 g). Finally, the organic solvents were evaporated, and the corresponding disulfides were obtained in high to excellent yields (88-98%). |
| 91% |
With dimethyl sulfoxide at 80 - 90℃; for 4h; |
4.6. General preparation of disulfides (9{z})
General procedure: An equimolar mixture of thiophenol (10{z}) and DMSO was heated at 80-90 °C for 4 h. The reaction was cooled to room temperature, diethyl ether was added and washed with water (×5). The organic phase was dried over anhydrous magnesium sulfate and evaporated to dryness in vacuo to give (9{z}). |
| 91% |
With 1,3-dibromo-5,5-dimethylimidazolidine-2,4-dione In chloroform at 25℃; for 0.0833333h; |
|
| 88% |
With bis(4-methoxyphenyl)telluride; 5,15,10,20-tetraphenylporphyrin In dichloromethane at 0℃; for 0.25h; Irradiation; |
|
| 85% |
With sodium hydrogensulfite; periodic acid In water at 20℃; for 1.66667h; |
|
| 71% |
With melamine hydrogen peroxide In acetonitrile for 0.17h; Reflux; |
|
|
With iodine In methanol |
|
|
With [K.18-crown-6][Br3]n In acetonitrile at 20℃; |
|
|
With 3,6-bis(dimethylamino)-9-(2,4,6-trimethylphenyl)-9H-telluroxanthen-9-ylium hexafluorophosphate; oxygen In chloroform-d1; water for 2h; Irradiation; |
|
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