Related Products of 102-52-3, These common heterocyclic compound, 102-52-3, name is 1,1,3,3-Tetramethoxypropane, its 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.
Example 6Preparation of Bromomalonaldehyde (9); De-ionized water (2.080 L) was added to a 12-L, four-neck flask under a nitrogen atmosphere and equipped with a thermocouple. Concentrated HCl (88 mL) was added to the water. Malonaldehyde bis-dimethylacetal (2006 mL, 2.0 kilogram (kg), 12.18 moles) was added dropwise over a period of 45 to 60 minutes while the temperature was maintained between 5 C. and 25 C. Bromine (1.912 g, 619 mL; 12 moles; 1 equivalent.) was added dropwise over 1 hour, while the temperature was maintained between 5 C. and 20 C. The reaction was monitored by HPLC for completion. After completion of the reaction (2 to 4 hours), the reaction mixture was concentrated on a rotary evaporator at 45 C. and 100 torr. The resultant mixture was stirred for 1 hour at room temperature, filtered, and washed with cold water (2¡Á1.0 liter). The isolated solids were dried in a forced-air dryer for 2 days. The weight of the product (9) obtained was 1.008 kg, with a 430 g second crop from the filtrate, giving a combined 76% yield. The second crop of crystals was obtained by concentrating the mother liquor to half its original volume and filtering off the resulting crystals. Mass spectrometry (M+H): 150.97 and 151.96 amu.
Statistics shows that 1,1,3,3-Tetramethoxypropane is playing an increasingly important role. we look forward to future research findings about 102-52-3.
Reference:
Patent; Wyeth; US2009/18332; (2009); A1;,
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