Phosgene → HCID 86623920, compound

Participants

Reaction Conditions

Reaction Steps

A 100 mL round-bottomed flask was fitted with a stirring bar and dropping funnel. To the reaction flask was added dichloromethane (30 mL) and the vessel was set to chill in an ice/water bath. To the flask was added 19% v/v phosgene in toluene (6 mL). 2-(3-piperidin-4-ylidenemethyl-phenoxy)-5-trifluoromethyl-pyridine hydrochloride (3.34 g, 9 mmol, from Example 1a, Step 5) was dissolved in a 15% v/v solution of diisopropylethylamine in dichloromethane and added to the chilled reaction flask slowly using the dropping funnel. Upon addition, the solution was stirred at 0° C. for 1 h. Upon completion of the reaction, the solvent and excess phosgene were removed in vacuo. A 0.2 M stock solution of the residue in dichloroethane was prepared for use in the next step (45 mL).

Provenance & Evidence