These common heterocyclic compound, 42726-73-8, name is tert-Butyl methyl malonate, 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. Formula: C8H14O4
EXAMPLE 125 Diethyl 2,2-Difluoroglutarate (b) Diethyl 2-ketoglutarate (a, 10.06 g, 49.74 mmol), methylene chloride (150 ml), and water (0.5 ml) were combined in a stainless steel bomb under N2 and cooled to -78. Sulfur tetrafluoride (~90 g, 833 mmol) was condensed in a polypropylene bottle at -78 and added to the reaction mixture. The bomb was sealed, then allowed to come to room temperature. After a total of 20 hrs, the bomb was vented through aqueous sodium hydroxide. The reaction mixture was worked up with methylene chloride, washing with aqueous sodium bicarbonate and brine. It yielded 11.38 g of crude yellow oil containing a white solid material. The white solid was filtered off and the oil distilled under reduced pressure through a Vigreux column. (bp 82-95, 5 mm). Total yield 6.27 g (57%) of the title compound as a light yellow oil. Silica gel tlc: Rf 0.47 in EtOAc:Hexane 1:3,
The synthetic route of tert-Butyl methyl malonate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; The University of Chicago; US4324730; (1982); A;,
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