Toluene → HCID 19424732, compound

Participants

Reaction Conditions

Reaction Steps

The remaining ⅔ of the reaction mixture (69.3%) was gradually stripped at elevated temperature and reduced pressure in the stainless steel reactor of unreacted toluene and TMEDA (ending conditions pot temperature 160° C. and 50 mmHg vacuum). The mixture was cooled to 100° C. and the reactor's content was transferred to the wash vessel previously heated to 85° C. and charged with 1700 g of fresh toluene. The TMEDA stripped product mixture was washed (3×300 ml) with deoxygenated water. Phase cuts were made at 80° C., and were rapid requiring little settling time. Water and any rag or emulsion was removed through the bottom drain valve. The temperature of the oil jacket was increased to 170° C. Residual moisture and toluene were distilled through a simple distillation head (1 atm.). When the pot temperature reached 161° C., the material was cooled and drained into a nitrogen-purged bottle (2918 g).

Provenance & Evidence