Method for synthesizing amide through nitrile hydrolysis
A technology of nitrile hydrolysis and amide, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, and the preparation of organic compounds, etc., to achieve the effects of low reaction temperature, broad development prospects, and good energy-saving effects
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Embodiment 1
[0023] Embodiment 1: benzamide
[0024]
[0025] Benzonitrile (103mg, 1mmol), [Cp*Rh(H 2 O) 3 ][OTf] 2 (3.0mg, 0.005mmol, 0.5mol%), acetaldehyde oxime (65mg, 1.1mmol) and water (1ml) were sequentially added to a 25ml Schlenk reaction flask. After the reaction mixture was reacted at 50°C for 6 hours, it was cooled to room temperature, water was removed by rotary evaporation, and the target product was obtained by column separation. Yield: 87%
[0026] 1 H NMR (500MHz, CDCl 3 )δ7.82(d,J=7.3Hz,2H,ArH),7.54-7.44(m,3H,ArH),6.09(br s,2H,NH 2 ); 13 C NMR (125MHz, CDCl 3 )δ169.7, 133.4, 131.9, 128.5, 127.3.
Embodiment 2
[0027] Embodiment 2:4-Methylbenzamide
[0028]
[0029]
[0030] 4-Methylbenzonitrile (117mg, 1mmol), [Cp*Rh(H 2 O) 3 ][OTf] 2 (3.0mg, 0.005mmol, 0.5mol%), acetaldehyde oxime (65mg, 1.1mmol) and water (1ml) were sequentially added to a 25ml Schlenk reaction flask. After the reaction mixture was reacted at 50°C for 6 hours, it was cooled to room temperature, water was removed by rotary evaporation, and the target product was obtained by column separation, yield: 87%
[0031] 1 H NMR (500MHz, DMSO-d 6 )δ8.13(br s,1H,NH),8.02-7.97(m,4H,ArH),7.55(br s,1H,NH),3.87(s,3H,CH 3 ); 13 C NMR (125MHz, DMSO-d 6 )δ168.0, 141.1, 131.5, 128.7, 127.5, 20.9.
Embodiment 3
[0032] Embodiment 3: 3,5-dimethylbenzamide
[0033]
[0034] 3,5-Dimethylbenzonitrile (131mg, 1mmol), [Cp*Rh(H 2 O) 3 ][OTf] 2 (3.0mg, 0.005mmol, 0.5mol%), acetaldehyde oxime (65mg, 1.1mmol) and water (1ml) were sequentially added to a 25ml Schlenk reaction flask. After the reaction mixture was reacted at 50°C for 6 hours, it was cooled to room temperature. , rotary evaporation to remove water, column separation to obtain the target product, yield: 84%
[0035] 1 H NMR (500MHz, DMSO-d 6 )δ7.86(br s,1H,NH),7.46(s,2H,ArH),7.22(br s,1H,NH),7.14(s,1H,ArH),2.29(s,6H,2xCH 3 ); 13 C NMR (125MHz, DMSO-d 6 )δ168.6, 137.5, 134.3, 132.7, 125.4, 21.0.
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