HCID 67247801, compound → HCID 67254163, compound

Participants

Reaction Steps

0.746 g of 4-bromo-2-(3-p-tolyl-2H-azirin-2-yl)pyridine obtained in step 13.2 is dissolved in the presence of 6.6 mg (0.052 mmol) of iron (H) chloride in 30 mL of 1,2-dimethoxyethane. The medium is then refluxed for 6 hours. A further 10 mg (0.078 mmol) of iron (II) chloride are then added and the mixture is refluxed again with stirring for 3 hours. The medium is then diluted with 50 mL of ethyl acetate and 50 mL of water. The organic phase is then recovered, dried over sodium sulfate and filtered. 2 g of silica are then added to the filtrate, followed by concentrating under reduced pressure. The powder obtained is used as a solid deposit for a chromatography on silica gel, eluting with a mixture of cyclohexane and ethyl acetate (85/15). 0.534 g (71%) of expected compound is recovered in the faun of a yellow powder.

Provenance & Evidence