Some common heterocyclic compound, 15568-85-1, name is 5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione, molecular formula is C8H10O5, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Quality Control of 5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione
A mixture of sulfone 5 (1.58g, 7.5mmol) and 15(558 mg, 3 mmol) in freshly distilled DMF (9 mL) was added to a mixture of HgCl2 (49mg, 0.18 mmol)and Mg (183mg, 7.5 mmol) in DMF (3 mL) at ambient temperature. The reaction was heated to 75 Cand stirred for an additional 3 h. The reaction was cooled to rt and quenched with 7M HCl. The reactionmixture was then heated to 110 C and stirred for an hour. The reaction mixture was cooled to rt andextracted with diethyl ether (3), dried over MgSO4 and concentrated under reduced pressure and dried toobtain crude carboxylic acid. The crude acid was dissolved in dry DMF and added to a round-bottomedflask containing anhydrous K2CO3 (830 mg, 6 mmol) after which benzyl bromide (0.7 mL, 6 mmol) wasadded. The mixture was stirred for 2 h and then diluted with water and extracted with diethyl ether (3),washed with brine and dried over MgSO4. The ethereal layer was concentrated under reduced pressure toobtain the crude ester
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 15568-85-1, its application will become more common.
Reference:
Article; Sakavuyi, Kaumba; Petersen, Kimberly S.; Tetrahedron Letters; vol. 54; 45; (2013); p. 6129 – 6132;,
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