Dichloromethane → HCID 86702583, compound

Participants

Reaction Steps

An anhydrous dichloromethane (323 mL) solution of the compound 7 (38.0 g) and triethylamine (44 mL) was cooled to around −60° C. in a dry ice-methanol bath, and mesyl chloride (15 mL) was added dropwise over about 20 minutes. The bath was changed to an ice bath, the mixture was stirred for 2 hours, and the reaction mixture was then added to cold water (600 mL), and extracted with a mixed solution of hexane (600 mL) and ethyl acetate (600 mL). The organic layer was washed with 1 M hydrochloric acid (290 mL) and a saturated saline (300 mL×3 times), dried with anhydrous sodium sulfate, and then concentrated to obtain a titled compound (44.7 g) having the following physical property values.

Provenance & Evidence