Dichloromethane → HCID 86624961, compound

Participants

Reaction Steps

To a stirred solution of 2.46 g (12.5 mmol) 4a and 50 ml dichloromethane were added 20.5 g (125 mmol) methyltriflate (Aldrich) drop wisely. The reaction mixture was refluxed for 2 days. The solvent was carefully substituted by dichloroethan. The reaction mixture was refluxed for 2 days and then cooled to room temperature. Diethylether was added. The desired compound precipitates and the solvent was decanted. The solid was washed extensively (ten times) with large amounts of diethylether. The solid was dried by use of oil pump vacuum and purified by (C-18) RP-column chromatography (acetonitril/water-gradient 1:99 to 80:20). The desired compound 4b was obtained in 80% yield (3.61 g, 10.0 mmol).

Provenance & Evidence