Hydrochloric Acid → HCID 86752469, compound

Participants

Reaction Steps

To a solution of the compound (26.7 g, 57 mmol) obtained in the item (c) inchloroform (50 ml), a 4-N hydrochloride in ethyl acetate (30 ml) is added at 0° C. The mixture is stirred for 3 hours and then the solvent isevaporated. The resulting residue was dissolved in dichloromethane (250 ml)and triethylamine (19 ml) is added. Then, a solution of methanesulfonyl chloride (7.9 g, 68 mmol) in dichloromethane (50 ml) is added at 0°C. and the mixture is stirred for 3 hours. The organic layer is washed oncewith a saturated sodium bicarbonate solution, water and saturated brine, successively, and then dried over sodium sulfate. The resulting residue ispurified with silica gel chromatography (hexane-ethyl acetate) to give 18.6g of the titled compound (73%).

Provenance & Evidence