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ChemicalBook CAS DataBase List 2-ACETYL-ISONICOTINONITRILE
37398-49-5

2-ACETYL-ISONICOTINONITRILE synthesis

3synthesis methods
4-Cyanopyridine

100-48-1

Acetoacetic Acid

541-50-4

2-ACETYL-ISONICOTINONITRILE

37398-49-5

Step 1: In a reaction flask containing a mixed solution of dichloromethane (1300 mL) and water (1100 mL) with 4-cyanopyridine (52 g, 0.5 mol), ammonium persulfate ((NH4)2S2O8) (170 g, 0.75 mol), silver nitrate (6.8 g, 0.04 mol), and aqueous sulfuric acid (40 mL, prepared from 98 mL of concentrated sulfuric acid (prepared with 400 mL of water). Subsequently, a solution of 3-oxobutanoic acid (110 g, 1.25 mol) in dichloromethane (100 mL) was added slowly and dropwise while keeping the reaction mixture at reflux. After refluxing the reaction for 2 h, the reaction mixture was alkalized with sodium carbonate powder to pH 8-9. The reaction mixture was filtered and the filtrate was extracted with dichloromethane (500 mL x 3). The organic phases were combined, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was recrystallized by ethanol to give 2-acetylisonicotinonitrile (52.0 g, 71.9% yield).

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Yield:37398-49-5 71.9%

Reaction Conditions:

with ammonium peroxydisulfate;sulfuric acid;silver nitrate in dichloromethane;water;Reflux;

Steps:

1 Step 1 : 2-Acetylisonicotinonitrile

Step 1 : 2-Acetylisonicotinonitrile To a solution of isonicotinonitrile (52 g, 0.5 mol) in dichloromethane (1300 mL) and water (1 100 mL) were added ammonium persulfate ((NH4)2S208) (170 g, 0.75 mol), silver nitrate (6.8 g, 0.04 mol) and aqueous sulfuric acid (40 mL, 98% sulfuric acid in 400 mL). A solution of 3-oxo-butyric acid (1 10 g, 1.25 mol) in dichloromethane (100 mL) was added dropwise while keeping the mixture refluxing. The reaction mixture was refluxed for 2 h. The resulting mixture was basified to pH -8-9 using sodium carbonate powder. The mixture was filtered and the filtrate was extracted with dichloromethane (500 mL x 3). The combined organics were dried over sodium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethanol to afford 2-acetylisonicotinonitrile (52.0 g, 71.9%).

References:

WO2013/150416,2013,A1 Location in patent:Page/Page column 117

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