Method for preparing 2-aryl-2,2-dimethyl methyl acetate
A technology of methyl dimethyl acetate and aryl acetic acid, which is applied in the field of organic synthesis, can solve problems such as high cost, difficult recycling, and increased process complexity, and achieve the effects of increased yield and simplified process
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Embodiment 1
[0060]Add 70mL of anhydrous tetrahydrofuran to a 250mL four-necked flask protected by nitrogen, then add 6.9g of sodium hydride, control the temperature to 10°C with an ice-water bath, and slowly add a mixture of 10g of p-bromophenylacetic acid and 30mL of anhydrous tetrahydrofuran dropwise at 10°C solution, after the dropwise addition, slowly return to room temperature for 0.5 hour reaction. Then lower the temperature to 10°C, slowly add 6.5g of dimethyl sulfate dropwise at 10°C to 20°C, heat to reflux for 2 hours after the addition, and when the reaction can no longer continue, use an ice-water bath to control the temperature to 10°C Still at 10°C-20°C, 7.3g of methyl iodide was slowly added dropwise, and after the dropwise addition was completed, it was heated to reflux for 1.5 hours until the reaction was complete. Quenched with water during monitoring, extracted with ethyl acetate, GC monitoring (see attached figure 1 ). After treatment, cool to room temperature, add 30...
Embodiment 2
[0062] Add 50mL of anhydrous N,N-dimethylformamide into a 250mL four-neck flask protected by nitrogen, then add 6.9g of sodium hydride, control the temperature to 15°C with an ice-water bath, and slowly add 10g of p-bromobenzene dropwise at 15°C The mixed solution of acetic acid and 30 mL of anhydrous N,N-dimethylformamide was slowly returned to room temperature for 0.5 hours after the dropwise addition. Then lower the temperature to 10°C, slowly add 6.5g of dimethyl sulfate dropwise at 10°C to 20°C, heat to reflux for 2 hours after the addition, and when the reaction can no longer continue, use an ice-water bath to control the temperature to 10°C Still at 10°C-20°C, 7.3g of methyl iodide was slowly added dropwise, and after the dropwise addition was completed, it was heated to reflux for 1.5 hours until the reaction was complete. Quenched with water while monitoring, extracted with ethyl acetate, monitored by GC. After-treatment, cool to room temperature, add 30 mL of water ...
Embodiment 3
[0064] Add 50mL of anhydrous 1,4-dioxane to a 250mL four-neck flask protected by nitrogen, then add 6.9g of sodium hydride, control the temperature to 20°C with an ice-water bath, and slowly add 10g of p-bromophenylacetic acid dropwise at 20°C With the mixed solution of 70mL of anhydrous 1,4-dioxane, slowly return to room temperature to react for 0.5 hours after the dropwise addition. Then lower the temperature to 10°C, slowly add 6.5g of dimethyl sulfate dropwise at 10°C to 20°C, heat to reflux for 2 hours after the addition, and when the reaction can no longer continue, use an ice-water bath to control the temperature to 10°C Still at 10°C-20°C, 7.3g of methyl iodide was slowly added dropwise, and after the dropwise addition was completed, it was heated to reflux for 1.5 hours until the reaction was complete. Quenched with water while monitoring, extracted with ethyl acetate, monitored by GC. After treatment, cool to room temperature, add 30 mL of water dropwise to the reac...
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