4-cyano-N methyl benzamide

Prepararation 4-cyano-N methyl benzamide.

A mixture of 4-bromo-N-ethyl-3-methylnenzamide (3.76 g, 16.5 mmol, can be synthesized according to the following reference Oxford, A. W.; et al EP 533266 (1993)), K4[Fe(CN)₆]-3H₂0 (2.09 g, 4.94 mmol), Na₂C0₃ (1.05 g, 9.89 mmol), Pd(OAc)₂ (75 mg, 0.33 mmol), l,4-diazabicyclo[2.2.2] octane (74 mg, 0.66 mmol), and DMA (20 mL) was maintained under N₂ atmosphere at 126-130°C for 7.5 hr. Afterward, the mixture was cooled to room temperature, diluted with EtOAc, stirred for 20 min, and filtered through diatomaceous earth. The filtrate was concentrated under reduce pressure, and the residue (5.52 g) was stirred in a mixture of Et₂0 (5 mL) and hexanes (10 mL). Afterward, the solid was collected by filtration, and washed with Et₂0 to form the title compound (2.53 g). The mother liquor was concentrated under reduce pressure, and the residue was stirred in a mixture of Et₂0 (2 mL) and hexanes (4 mL) to form an additional amount of the compound (0.265 g) as a solid. Both batches were combined (2.80 g, 97%). 

¾ NMR (300 MHz, CDC1₃) δ ppm 2.59 (s, 3H), 3.03 (d, J = 4.9 Hz, 3H), 6.17 (br s, 1H), 7.61 (dd, J = 8.2, 1.5 Hz, 1H), 7.66 (d, J = 8.0 Hz, 1H), 7.73 (s, 1H).

http://www.google.com/patents/WO2014117274A1?cl=en

vietnam

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