(Z)-3-dimethylamino-alpha-4'-substituted benzene sulfydryl-alpha, beta-unsaturated aromatic amide compound and preparation method thereof
A technology of phenylmercaptoacetyl chloride compound and dimethylamino group, which is applied in the synthesis field of amide organic compounds and achieves the effects of few reaction steps, high purity and simple reaction process
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Embodiment 1
[0022] (E )-N'-(4-ethoxyphenyl)-N, N-dimethylaminoformamidine (7.69 g, 0.04 mol), carbon tetrachloride (30 ml), potassium carbonate (6.91 g, 0.05 mol) and a magneton into a 100 ml single-necked round bottom flask, start the magnetic stirrer, and place the reaction bottle at 5 o C in a cold bath. 2-(4'-Chlorophenylmercapto)acetyl chloride (13.3 g, 0.06 mol) was slowly added dropwise with a syringe, and the whole dropping process lasted about 50 minutes. After the addition was complete, the reaction mixture was stirred overnight at room temperature. The solvent was removed by rotary evaporation. Ethyl acetate (20 ml) and water (20 ml) were then added to the reaction flask and stirred for 10 minutes, transferred to a separatory funnel and the lower inorganic phase was separated. The inorganic phase was extracted with ethyl acetate (10 ml). The organic phases were combined and washed with saturated brine (20 mL) and water (20 mL), respectively. The organic phase was dri...
Embodiment 2
[0024] (E)-N'-(4-ethoxyphenyl)-N, N-dimethylaminoformamidine (3.84 g, 0.02 mol), toluene (20 ml), sodium hydroxide (0.8 g, 0.02 mol) and a magnetron into a 100 ml single-necked round bottom flask, start the magnetic stirrer, and place the reaction bottle at -45 oC in a cold bath. 2-(4'-chlorophenylmercapto)acetyl chloride (6.6 g, 0.03 mol) was slowly added dropwise with a syringe, and the whole dropping process lasted for about 35 minutes. After the addition was complete, the reaction mixture was stirred overnight at room temperature. The solvent was removed by rotary evaporation. Ethyl acetate (20 ml) and water (20 ml) were then added to the reaction flask and stirred for 10 minutes, transferred to a separatory funnel and the lower inorganic phase was separated. The inorganic phase was extracted with ethyl acetate (10 ml). The organic phases were combined and washed with saturated brine (20 mL) and water (20 mL), respectively. The organic phase was dried over anhyd...
Embodiment 3
[0026] (E)-N'-(4-ethoxyphenyl)-N, N-dimethylaminoformamidine (3.84 g, 0.02 mol), ethyl acetate (20 ml), sodium phosphate (4.92 g, 0.03 mol ) and a magneton into a 100 ml single-necked round bottom flask, start the magnetic stirrer, and place the reaction bottle at 0 o C in an ice-water cooling bath. Then 2-(4'-chlorophenylmercapto)acetyl chloride (8.84 g, 0.04 mol) was slowly added dropwise with a syringe, and the whole dropping process continued for about 40 minutes. After the dropwise addition of 2-(4'-chlorophenylmercapto)acetyl chloride, the reaction mixture was stirred overnight at room temperature. The solvent was removed by rotary evaporation. Ethyl acetate (20 ml) and water (20 ml) were then added to the reaction flask and stirred for 10 minutes, transferred to a separatory funnel and the lower inorganic phase was separated. The inorganic phase was extracted with ethyl acetate (10 ml). The organic phases were combined and washed with saturated brine (20 mL) and wat...
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