Ethyl Bromide → HCID 54303576, compound

Participants

Reaction Conditions

Reaction Steps

33.2 g (0.240 mol) of potassium carbonate are introduced into 100 ml of dimethylformamide and cooled to -5° C. 37.5 g (0.114 mol) of 2-chloro-3,5-dinitrobenzoic acid (75% with 25% water) dissolved in 120 ml of dimethylformamide are then added over a period of 20 minutes during which time the internal temperature is maintained at from -5° to 0° C. 8.9 ml (0.12 mol) of ethyl mercaptan in 20 ml of dimethylformamide are then added dropwise at -8° C. over a period of 20 minutes. The batch is then stirred for one hour at that same temperature and afterwards the temperature is raised to room temperature over a period of 19 hours. 9.0 ml (0.12 mol) of ethyl bromide in 20 ml of dimethylformamide are then added dropwise over a period of 10 minutes and the reaction mixture is subsequently stirred for 24 hours at room temperature and then poured onto 500 ml of ice/water, stirred and filtered. The material obtained by filtering with suction is washed with water and then dried at room temperature in vacuo and in the presence of phosphorus pentoxide.

Provenance & Evidence