Phosphorus sulfide (P2S5) → HCID 12056675, compound

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Reaction Steps

In a 250 ml two-necked flask, N-(6-chloro-3-pyridylmethyl)-N-methyl-2-methylpropanamide (6.80 g, 30.0 mmol) is dissolved in 120 ml of benzene, 1.47 g (3.3 mmol) of phosphorus pentasulfide are added and the mixture is heated at reflux for 1.5 hours. After this period of time, the mixture is cooled to room temperature and filtered, and the filtrate is concentrated under reduced pressure using a rotary evaporator. To increase the yield on the same day, the product should be subjected to silica gel column chromatography using the mobile phase dichloromethane/diethyl ether 10/3; Rf=0.8.

Provenance & Evidence