[acetyloxy(phenyl)methyl] acetate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 61 g of benzal diacetate, 44.6 g of 4-methylsalicylic acid and 45 ml of acetic acid are combined and 5 drops of concentrated sulfuric acid are added and the mixture is heated under reduced pressure, allowing acetic acid to distill off. When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture is allowed to cool, diluted with ether and the ether solution washed with potassium carbonate solution, sodium bisulfite solution and dried over sodium sulfate. The ether is removed in vacuo and the resulting solid crystallized from ethyl acetate/hexane to give 7-methyl-1,3-benzodioxane-4-one. the mixture is heated under reduced pressure to distill off When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture to cool diluted with ether the ether solution washed with potassium carbonate solution, sodium bisulfite solution dried over sodium sulfate The ether is removed in vacuo the resulting solid crystallized from ethyl acetate/hexane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 61 g of benzal diacetate, 44.6 g of 4-methylsalicylic acid and 45 ml of acetic acid are combined and 5 drops of concentrated sulfuric acid are added and the mixture is heated under reduced pressure, allowing acetic acid to distill off. When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture is allowed to cool, diluted with ether and the ether solution washed with potassium carbonate solution, sodium bisulfite solution and dried over sodium sulfate. The ether is removed in vacuo and the resulting solid crystallized from ethyl acetate/hexane to give 7-methyl-1,3-benzodioxane-4-one. the mixture is heated under reduced pressure to distill off When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture to cool diluted with ether the ether solution washed with potassium carbonate solution, sodium bisulfite solution dried over sodium sulfate The ether is removed in vacuo the resulting solid crystallized from ethyl acetate/hexane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a manner similar to that in Example 1, m-xylylene dichloride was converted into m-diacetoxymethylbenzene at 97° to 101° C. in 3 hours by use of a reactant mixture comprising 100 parts of m-xylylene dichloride (97.6% purity), 100 parts of anhydrous sodium acetate, 125 parts of monochlorobenzene, and 2 parts of triethylamine. To the reaction mixture was added 250 parts of warm water to dissolve the by-product sodium chloride. The mixture was left standing at 80° C. to allow it to settle in two layers. To the monochlorobenzene layer which had been freed from the catalyst amine by removing in the same manner as in Example 1, were added 46 parts of sodium hydroxide and 310 parts of water to allow the saponification to proceed at 94° C. for 2 hours. After saponification, the reaction mixture was neutralized with 3N hydrochloric acid and left standing at 82° C. to allow the mixture to settle in two layers. The aqueous layer containing m-xylylene glycol, was added at 80° C. 50 parts of monochlorobenzene to extract impurities. After separation, m-xylylene glycol was extracted from the purified aqueous layer with n-butyl acetate in the same way as in Example 1. The n-butyl acetate layers obtained by repeating batchwise extraction three times were combined, distilled to recover ethyl acetate, and dried in vacuo to obtain 76.0 parts of m-xylylene glycol (melting point, 53.5° - 55° C.) in a yield of 98.7%. The mixture was left standing at 80° C. by removing in the same manner as in Example 1 were added 46 parts of sodium hydroxide and 310 parts of water left standing at 82° C. The aqueous layer containing m-xylylene glycol was added at 80° C 50 parts of monochlorobenzene to extract impurities After separation, m-xylylene glycol was extracted from the purified aqueous layer with n-butyl acetate in the same way as in Example 1 The n-butyl acetate layers obtained extraction three times distilled to recover ethyl acetate dried in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 61 g of benzal diacetate, 44.6 g of 4-methylsalicylic acid and 45 ml of acetic acid are combined and 5 drops of concentrated sulfuric acid are added and the mixture is heated under reduced pressure, allowing acetic acid to distill off. When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture is allowed to cool, diluted with ether and the ether solution washed with potassium carbonate solution, sodium bisulfite solution and dried over sodium sulfate. The ether is removed in vacuo and the resulting solid crystallized from ethyl acetate/hexane to give 7-methyl-1,3-benzodioxane-4-one. the mixture is heated under reduced pressure to distill off When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture to cool diluted with ether the ether solution washed with potassium carbonate solution, sodium bisulfite solution dried over sodium sulfate The ether is removed in vacuo the resulting solid crystallized from ethyl acetate/hexane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 61 g of benzal diacetate, 44.6 g of 4-methylsalicylic acid and 45 ml of acetic acid are combined and 5 drops of concentrated sulfuric acid are added and the mixture is heated under reduced pressure, allowing acetic acid to distill off. When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture is allowed to cool, diluted with ether and the ether solution washed with potassium carbonate solution, sodium bisulfite solution and dried over sodium sulfate. The ether is removed in vacuo and the resulting solid crystallized from ethyl acetate/hexane to give 7-methyl-1,3-benzodioxane-4-one. the mixture is heated under reduced pressure to distill off When the theoretical amount of acetic acid is collected (about 2.5 hours) the mixture to cool diluted with ether the ether solution washed with potassium carbonate solution, sodium bisulfite solution dried over sodium sulfate The ether is removed in vacuo the resulting solid crystallized from ethyl acetate/hexane