ChemicalBook CAS DataBase List 4-Cyanopyridine

4-Cyanopyridine synthesis

9synthesis methods

Product Name:4-Cyanopyridine
CAS Number:100-48-1
Molecular formula:C6H4N2
Molecular Weight:104.11

4-Cyanopyridine is synthesised by the reaction of 4-methylpyridine with ammonia and air in the presence of a catalyst. The specific synthesis steps are as follows:
4-Methylpyridine and ammonia vaporisation preheating to 180-330°C, then into the mixing tank and air mixing uniformly, into the fixed-bed reactor by the top of the fixed-bed reactor after the distribution of the catalyst-filled reactor, the control of the reaction temperature in the range of 330-450 ° C, the reaction head pressure is controlled in the range of 0.020-0.070 KPa, the reaction temperature is controlled by molten salts, the reaction gas after the end of the reaction After the reaction, the reaction gas was condensed to sub-zero fractionation to obtain the crude product of 4-cyanopyridine, and the crude product was distilled to obtain the finished product of 4-cyanopyridine. The conversion rate of 4-methylpyridine was above 99%, and the yield of 4-cyanopyridine was above 98%.
4-Cyanopyridine synthesis

872-85-5 Synthesis

872-85-5
492 suppliers
$10.00/1g

100-48-1
501 suppliers
$8.00/25g

Yield:100-48-1 96%

Reaction Conditions:

with ammonium hydroxide;sodium peroxodisulphate;sodium iodide;iron(II) chloride in 1,2-dichloro-ethane at 20 - 50; for 16 h;

Steps:

General procedure for the synthesis of nitriles

General procedure: To a solution of aldehydes 1 (3 mmol) in 1,2-dichloroethane (10 mL) was added FeCl₂(0.3 mmol), Na₂S₂O₈ (4.5 mmol), NaI (0.15 mmol), and NH₃.H₂O (9 mL) at room temperature. After the mixture was stirred at 50 °C for 16 hours, it was poured into water (30 mL) and extracted with DCM (3 × 30 mL). The combined organic extracts were washed with brine and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure. The crude product was purified by column chromatography on silica gel to afford the product 2.

References:

Chen, Han;Sun, Sijia;Xi, Haoying;Hu, Kaifang;Zhang, Ning;Qu, Jingping;Zhou, Yuhan [Tetrahedron Letters,2019,vol. 60,# 21,p. 1434 - 1436] Location in patent:supporting information

696-54-8 Synthesis