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ChemicalBook CAS DataBase List 4-Pyridyl acetone

4-Pyridyl acetone synthesis

12synthesis methods
-

Yield:6304-16-1 74.3%

Reaction Conditions:

Stage #1: picoline;acetyl chloride in chloroform at 30 - 35; for 2 h;Cooling with ice;
Stage #2: with sodium hydroxide in chloroform at 30; for 2 h;Temperature;

Steps:

4 Example four

In a 1000mL three-neck flask,Added 4-methylpyridine 93.0g (1.0mol), chloroform 500mL,In an ice water bath, 80.0 g (1.0 mol) of acetyl chloride was added dropwise at a controlled temperature of 35°C.After completion of the addition, the temperature was raised to 30°C and the reaction was continued for 2 hours. After completion of the reaction, an aqueous saturated sodium carbonate solution was added dropwise to the system under ice-cooling to adjust the pH to 5-7, and then 133.4 g (1 mol of sodium hydroxide) of 30 wt% sodium hydroxide solution was added and the reaction was stirred at 30°C for 2 hr. Reaction is completed, stratification, removal of water layer,Drying with anhydrous sodium sulfate, After recovering the solvent, vacuum distillation was performed to collect 100.3 g of a fraction of 100-105°C/200kPa.That is 1-(4-pyridyl)-2-propanone,HPLC: 98.4%, yield 74.3%.

References:

CN104387320,2018,B Location in patent:Paragraph 0048; 0052; 0056; 0059; 0060; 0064

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