Synthesis of 4-substrated aryl-1-benzenesulfonyl-3-butylene-2-one
A technology of benzenesulfonyl and chemical synthesis, applied in the direction of chemical instruments and methods, organic chemistry, and preparation of organic compounds, can solve the problems of unfavorable industrial production and harsh synthesis conditions, and achieve the convenience of industrial production, less discharge of three wastes, Facilitate the control effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0025] Example 1: Preparation of 4-phenyl-1-benzenesulfonyl-3-buten-2-one
[0026] The molar amount of feeding is: 0.1 mol of benzaldehyde, 0.5 mol of acetone, 0.1 mol of brominated reagent, and 0.2 mol of sodium benzenesulfinate.
[0027] The condensation reaction time is 2 hours, the concentration of inorganic alkali sodium hydroxide is 5%, the bromination temperature is 15° C., and the nucleophilic reaction time is 4 hours.
[0028] Proceed as follows:
[0029] (1) Add acetone and benzaldehyde to 50ml of water, add dropwise 5ml of sodium hydroxide aqueous solution to the mixed solution while stirring, continue to stir for 2 hours, add dilute hydrochloric acid until the solution is acidic, separate and distill under reduced pressure, collect 110~ 120℃ / 5mmHg distillate to get condensation products;
[0030] (2) Add dissolved Ph to the condensation product 3 P + CH 2 CH 2 COOHBr 3 - THF, heated and kept at 15°C until the solution was brown, left to stand, and a large a...
Embodiment 2
[0034] Example 2: Preparation of 4-m-methylphenyl-1-benzenesulfonyl-3-buten-2-one
[0035] The molar amount of feeding is: 0.1 mol of m-tolualdehyde, 2.0 mol of acetone, 0.5 mol of brominated reagent, and 0.7 mol of sodium benzenesulfinate.
[0036] The condensation reaction time is 8 hours, the concentration of inorganic alkali sodium carbonate is 15%, the bromination temperature is 70° C., and the nucleophilic reaction time is 12 hours.
[0037] Reaction steps are with embodiment 1.
[0038] The yield of condensation reaction is 76%; the yield of bromination reaction is 77%; the yield of nucleophilic reaction is 91%.
Embodiment 3
[0039] Example 3: Preparation of 4-p-tert-butylphenyl-1-benzenesulfonyl-3-buten-2-one
[0040] The molar amount of feeding is: 0.1 mol of p-tert-butylbenzaldehyde, 1.0 mol of acetone, 0.3 mol of brominated reagent, and 0.4 mol of sodium benzenesulfinate.
[0041] The condensation reaction time is 4 hours, the concentration of inorganic alkali potassium hydroxide is 8%, the bromination temperature is 30° C., and the nucleophilic reaction time is 8 hours.
[0042] Reaction steps are with embodiment 1.
[0043] The yield of condensation reaction is 76%; the yield of bromination reaction is 76%; the yield of nucleophilic reaction is 91%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More