Methyl iodide → HCID 54000078, 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) in 110 ml of dimethylformamide are then added over a period of 20 minutes, during which time the internal temperature is maintained at from -7° to -3° C. 11.0 ml (0.114 mol) of isopropyl mercaptan (97%) in 20 ml of dimethylformamide are then added dropwise at from -8° to -1° C. over a period of 45 minutes. The batch is then stirred for one hour at 0° C. and the temperature is then raised to 25° C. over a period of 24 hours. 7.5 ml (0.12 mol) of methyl iodide are then added dropwise at room temperature over a period of 30 minutes. The reaction mixture is subsequently stirred for 16 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 dried at room temperature.

Provenance & Evidence