Pyridine → HCID 18978176, compound

Participants

Reaction Steps

A mixture of 2-iso-propylphenol (10.0 g, 73.4 mmol) in trichloroethylene (600 mL) is added dropwise to a 0°-4° C. mixture of thiophosphoryl chloride (18.63 g, 110 mmol) and anhydrous pyridine (8.70 g, 110 mmol) in trichloroethylene (250 mL) over a 1 hour period under a nitrogen atmosphere. The resultant reaction mixture is stirred at 0°-4° C. for 2 hours, is warmed to room temperature and then is stirred at room temperature for 12 hours. A white solid gradually precipitates. The white solid is filtered from the reaction mixture. The resultant reaction mixture is concentrated in vacuo to a residue. Successive aliquots of toluene (200 mL) are added to the residue and then separately evaporated in vacuo to give (2-iso-propylphenyl)-thiophosphoryl dichloride which can be used directly without further purification as the starting material for Example 27.

Provenance & Evidence