Reference of 796851-03-1 , The common heterocyclic compound, 796851-03-1, name is 2,5-Dichloro-4-iodopyridine, molecular formula is C5H2Cl2IN, 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.
a) A mixture of 2,5-dichloro-4-iodopyridine (0.4Og, 1.46 mmol), 7-amino-2-methyl-4- (4-propan-2-ylpiperazin-l-yl)-3H-isoindol-l-one (0.421 g, 1.46 mmol), 9,9-dimethyl-4,5- bis(diphenylphosphino)xanthene (0.051 g, 0.09 mmol), cesium carbonate (0.952 g, 2.92 mmol) and palladium(II) acetate (0.013 g, 0.06 mmol) was suspended in DMA (15 mL). The mixture was heated at 1000C for 1 hour in a microwave reactor and then allowed to cool to room temperature. The mixture was loaded onto an SCX column and the product eluted first with MeOH and then with a 7M solution of NH3 in MeOH. Fractions containing product were combined and evaporated to afford 7-[(2,5-dichloropyridin-4- yl)amino]-2-methyl-4-(4-propan-2-ylpiperazin-l-yl)-3H-isoindol-l-one (0.630 g, 99% yield); 1H NMR spectrum: (300 MHz, DMSO) delta 1.01 – 1.18 (3H, d), 2.60 – 2.64 (4H, m), 3.04 – 3.09 (5H, m), 4.51 (2H, s), 7.16 (IH, d), 7.29 (IH, s), 7.50 (IH, d), 8.28 (IH, s), 9.59 (IH, s); Mass spectrum: m/z (ESI+) (M+H)+ = 434.0 and 436.0 and 438.0.
The synthetic route of 796851-03-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2009/153589; (2009); A1;,
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