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ChemicalBook CAS DataBase List Isonicotinamide
1453-82-3

Isonicotinamide synthesis

13synthesis methods
synthesis of isonicotinamide: In 6g tert-amyl alcohol, add 100mg ferric oxide, 100mg cobalt tetroxide and 100mg manganese dioxide (mass percentage in the mixture: 4.6%), 60mg 4-cyanopyridine (mass percentage in the mixture: 0.91%), 200uL Water (mass percentage in the mixture: 3.0%), mix well; react at 80°C for 24 hours, the conversion rate of 4-cyanopyridine is 99.0%, and the selectivity of the corresponding Isonicotinamide is 99.0%.
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Yield:1453-82-3 95%

Reaction Conditions:

Stage #1: pyridine-4-carboxylic acidwith chloroformic acid ethyl ester;triethylamine in tetrahydrofuran at 0; for 0.5 h;
Stage #2: with ammonium chloride in tetrahydrofuran;water at 0; for 0.5 h;

Steps:

4.2.11 4.2. Typical procedure for the primary amidation of 3-phenylpropanoic acid 1a with NH4Cl

General procedure: To a colorless solution of 75mg (0.50mmol) of 3-phenylpropanoic acid 1a in 10mL of THF were added at 0°C 67μL (0.70mmol, 1.4equiv) of ClCO2Et and 209μL (1.5mmol, 3.0equiv) of Et3N.
After stirring for 30min at 0°C, 0.75 ml of a 1.0M aqueous solution of NH4Cl (0.75mmol, 1.5equiv) was added at 0°C to the colorless suspension.
The mixture was stirred for 30min at 0°C and 5mL of H2O was added to the resulted mixture.
The colorless clear solution was extracted with 30mL of EtOAc and the aqueous layer was extracted with 20mL of EtOAc.
The organic layers were combined, washed with 5mL of brine, and dried over anhydrous MgSO4.
The crude product was chromatographed on silica gel with EtOAc to afford 72mg (96% yield) of 3-phenylpropanamide 2a. 4.2.11
Isonicotinamide 2k
58?mg (95%); colorless solid; mp: 151-153?°C; 1H NMR (400?MHz, DMSO-d6): δ 7.73 (br, 1H, NHA), 7.76, 8.72 (d, d, J?=?6.0, 6.0?Hz, 2H, 2H, pyridyl), 8.25 (br, 1H, NHB); 13C NMR (100?MHz, DMSO-d6): δ 121.3, 141.2, 150.1, 166.2; IR (KBr, vmax/cm-1)?=?3334 (CONH), 1684 (CON), 1624 (CON); HRMS (ESI-TOF): Calcd for C6H7N2O (M+H)+: 123.0553, found: 123.0529.

References:

Ezawa, Tetsuya;Kawashima, Yuya;Noguchi, Takuya;Jung, Seunghee;Imai, Nobuyuki [Tetrahedron Asymmetry,2017,vol. 28,# 12,p. 1690 - 1699]

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