Methane → HCID 19890947, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 4 g (0.0132 mol) 2-(3-picolylseleno)benzoic acid (from Example 2) and 4.4 ml triethylamine in 40 ml dichloromethane, that has been cooled to 0° C., is added in one portion 3.5 g (0.0132 mol) bis(2-oxo-3-oxazolidinyl)-phoshoryl chloride. After 15 minutes 1.3 g (0.0138 mol) 4-aminopyridine is added and the mixture stirred at 0° C. for 3.5 hours. It is then extracted twice with 100 ml portions of water, the organic phase dried over sodium sulfate and the solvent removed. The residue is taken up in 60 ml 2-propanol and treated with 10 ml 15% HCl in 2-propanol. The solid product that results is dissolved in 50 ml H2O and treated with 1 g active charcoal, stirred at room temperature for 15 minutes and then filtered. Acetone is added dropwise to the filtrate until the solution remains turbid. The crystals that are formed are filtered off after 2 hours and dried.

Provenance & Evidence