A kind of preparation method of disulfide compounds
A compound, disulfide technology, applied in the field of preparation of disulfide compounds, to achieve the effect of cheap raw materials, mild reaction conditions, and simple operation
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0016] The preparation method of a kind of disulfide compound comprises the following steps:
[0017] Disperse the carboxylic acid with structure (I) and sodium sulfide in a solvent, add tert-butyl nitrite to the above mixture, and then heat and stir to obtain the disulfide compound of the present invention with structure (II) : carboxylic acid with structure (I) and sodium sulfide are dispersed in a solvent, tert-butyl nitrite is added in the above mixture, and then the disulfides of the present invention with structure (II) can be obtained by heating and stirring Compound: the R is 4-chloro, 4-methyl, 3,6-dichloro-2-methoxy, 4-methoxy, 3,5-dimethoxy, 3-methyl-4 -nitro, 3-methoxy, 2-methoxy, 4-trifluoromethyl, 4-fluoro, 4-iodo, 4-bromo, 2-methyl-3-nitro, 4-cyano, 4-cyanomethyl, 4-ethyl, 4-acetylamino or 2-acetylamino.
[0018]
[0019] The solvent is N,N-dimethylacetamide, toluene, N,N-dimethylformamide, acetone, p-xylene, 1,4-dioxane, 1,2-dichloroethane , N-methylpyrro...
Embodiment 1
[0025] Add 1mmol p-toluic acid, 2mmol sodium sulfide, 3mmol tert-butyl nitrite in a clean and dry 50ml Schlenk pressure-resistant reaction tube, then add 10ml toluene, seal the reaction tube and place it in an oil bath at 100°C The reaction was heated in the pot for 10 hours. After the reaction, the mixture was spin-dried by a rotary evaporator, and the resulting residue was separated by a silica gel column with n-hexane as the eluent. The target product obtained was a white powder solid, which was analyzed by H NMR and C NMR , it was confirmed that the target product was p-toluene disulfide, and the yield was 89%.
[0026] The proton nuclear magnetic resonance spectrum of the product prepared in this embodiment is as follows: Figure 1a As shown, the carbon NMR spectrum is shown as Figure 1b shown.
Embodiment 2
[0028] Add 1mmol of p-toluic acid, 1mmol of sodium sulfide, 4mmol of tert-butyl nitrite in a clean and dry 50ml Schlenk pressure-resistant reaction tube, and then add 10ml of acetone, seal the reaction tube and place it in an oil bath at 120°C Heat reaction in the pot for 8 hours. After the reaction, the mixture was spin-dried by a rotary evaporator, and the resulting residue was separated by a silica gel column with n-hexane as the eluent. The target product obtained was a white powder solid, which was analyzed by H NMR and C NMR , it was confirmed that the target product was p-toluene disulfide, and the yield was 82%.
[0029] The proton nuclear magnetic resonance spectrum of the product prepared in this embodiment is as follows: Figure 1a As shown, the carbon NMR spectrum is shown as Figure 1b shown.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More