ChemicalBook CAS DataBase List 2-(2-THIENYL)PYRIDINE

2-(2-THIENYL)PYRIDINE synthesis

12synthesis methods

Product Name:2-(2-THIENYL)PYRIDINE
CAS Number:3319-99-1
Molecular formula:C9H7NS
Molecular Weight:161.22

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Yield: 77.36%

Reaction Conditions:

with cobaltocene in tetrahydrofuran at 140 - 190; under 975.098 - 14251.4 Torr; for 2 h;Autoclave;Inert atmosphere;Pressure;Temperature;

Steps:

5
Was added to the autoclave cobaltocene tetrahydrofuran solution (content 13%) 30g, the autoclave was sealed, evacuated, purged with nitrogen twice, and then pumped into the 2-cyano-thiophene 55.6g (purity 98%)And anhydrous tetrahydrofuran 100ml of the mixed solution, closed autoclave, vacuum, and then access to nitrogen, ventilation 2 times, after the access to acetylene gas to 0.13MPa, slowly stirring up to 140 , the temperature was stable,At this temperature continue to enter the acetylene gas 1.1MPa, stop ventilation, the reaction will automatically heat up to 190 and boost to 1.9MPa, stirring reaction 2 hours, System automatically cooling down when the pressure step down to 1.1MPa, open the cooling water, cooling to 40 below, discharge, concentrated recovery of tetrahydrofuran, the residue by adding water 200ml, add 30% hydrochloric acid PH1, add toluene for 30 minutes , The toluene layer, the water layer, the water layer and then 30% of the liquid alkali PH13, with 300ml toluene × 2 extraction, the organic phase washed twice, concentrated recovery of toluene, the residue by adding 80ml of methanol, a little activated carbon, heating and stirring The residue was decolored for 30 minutes and filtered to obtain a filtrate, and the temperature was lowered below 0 ° C to obtain 62.8 g of a white solid, 99.3% pure and a yield of 77.36%.

References:

Lianyungang Hongye Fine Chemical Co.,Ltd.;Meng, Mingfei;Wu, Shuiliang CN106380466, 2017, A Location in patent:Paragraph 0025; 0027