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ChemicalBook CAS DataBase List 4-Acetoxy-3-acetoxymethylacetophenone
24085-06-1

4-Acetoxy-3-acetoxymethylacetophenone synthesis

6synthesis methods
-

Yield:24085-06-1 93.6%

Reaction Conditions:

Stage #1: formaldehyd;4-Hydroxyacetophenonewith dimethyl amine in water at 40; for 8 h;
Stage #2: acetic anhydride at 110; for 4 h;

Steps:

3 Example 3: Preparation of 2-acetoxy-5-acetylbenzyl acetate (2)

To a 500 mL three-necked flask was added 13.5 g (110 mmol) of 33% aqueous dimethylamine solution,Hydroxyacetophenone 7.5 g (55 mmol),Paraformaldehyde 10 g (110 mmol),The temperature was adjusted to 40 ° C,Stir for 8 h.5N sulfuric acid (45.6 g) was added slowly,Followed by adjusting the pH to 7.0-7.5 with 27% aqueous ammonia solution,Then extracted with toluene (50 mL x 3)Combine organic phase,Saturated brine washing,Decompressed to a half volume (i.e., a solvent that directly reacts with toluene as a subsequent reaction)Acetic acid was added to 14 g (138 mmol)And refluxed at 110 ° C for 4 h.Cooled to room temperature,Washed with 10% sodium carbonate solution,Dried over anhydrous sodium sulfate,Concentrated under reduced pressure,To give 14.3 g of 2-acetoxy-5-acetylbenzyl acetate,The yield was 93.6%.

References:

CN106278910,2017,A Location in patent:Paragraph 0064; 0065; 0066; 0067; 0068; 0069; 0070-0081

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