Reference of 28868-76-0, A common heterocyclic compound, 28868-76-0, name is Dimethyl 2-chloromalonate, molecular formula is C5H7ClO4, 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.
To a suspension of K2CO3 (49.3 G) in acetone (100 ml) a solution of 2-chloro-5- methoxy-phenol (37.7 G, boiling point 83-86C, 13 mbar, [9]) was added dropwise at 40C. The dropwise addition of dimethyl CHLOROMALONATE (43.6 G) in acetone (100 ml) followed. The mixture was refluxed for 16 h before the solvent was removed under reduced pressure. The residue was taken up in water (400 ML) and extracted twice with DCM (400 ML). The organic extracts were dried over MGS04 and evaporated. Upon treatment of the oily residue with diethyl ether, the product crystallised. The crystals were collected, washed with a mixture of diethyl ether and hexane and dried to give 2- (2-chloro-5-methoxy-phenoxy)-malonic acid dimethyl ester (53.73 g) as white crystals. (CDC13) : 3.76 (s, 3H), 3.86 (s, 6H), 5.20 (s, 1 H), 6.53-6. 58 (m, 2H), 7.24-7. 29 (m, 1 H).
The synthetic route of 28868-76-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ACTELION PHARMACEUTICALS LTD; WO2004/50640; (2004); A1;,
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