반응 #48526

반응 방정식

2-chloro-3-cyanopyridine

potassium carbonate

benzyl mercaptan

→

2-(phenyl methyl thio)-3-cyanopyridine

용매

dimethyl formamide

dimethyl formamide

반응 조건

후처리

1. 1
   기타to obtain a suspension
2. 2
   기타Then, the reaction mixture was reacted at 120-130° C. for about 1.5 hours
3. 3
   온도Afterwards, heating
4. 4
   기타reaction mass
5. 5
   기타the room temperature
6. 6
   기타Inorganic cake was separated by filtration
7. 7
   workup.DISTILLATIONDimethyl formamide was distilled under reduced pressure
8. 8
   workup.WAITthe residue left

실험 절차

85 g of 2-chloro-3-cyanopyridine, 98.2 g potassium carbonate anhydrous powder and 600 g of dimethyl formamide were mixed to obtain a suspension. To this suspension, a solution of 79.2 g benzyl mercaptan in 250 ml dimethyl formamide was added dropwise over a period of approx. 3 hours at 80-90° C. The reaction mass was agitated for 2 hours at the same temperature. The temperature was slowly raised to 120° C. Then, the reaction mixture was reacted at 120-130° C. for about 1.5 hours. Afterwards, heating was stopped and reaction mass was allowed to attain the room temperature. Inorganic cake was separated by filtration. Dimethyl formamide was distilled under reduced pressure, and the residue left at bottom was 2-(phenyl methyl thio)-3-cyano pyridine 150 g, sufficiently pure to be used in the next step.

출처