Sodium hydride → HCID 18520400, compound

Participants

Reaction Steps

A DMF solution (50 ml) of 16.7 g of 2,2-dimethoxyethanol was added to dry DMF (60 ml) suspension of 4.32 g of sodium hydride at room temperature over 20 minutes. After 1 hour of stirring at room temperature, the reaction solution was cooled to 0° C., mixed with a DMF (20 ml) solution of 23.9 g of 2,5-difluoronitrobenzene and then stirred at 0° C. for 1 hour. The reaction solution was poured into 700 ml of ice water and extracted twice with a hexane-ethyl acetate (9:1) mixed solvent. The organic layer was washed with water and saturated brine in that order and dried with anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure to obtain 35.88 g of the title compound as a light red oil.

Provenance & Evidence