Toluene → HCID 19424732, compound

Temperature

100 °C

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).

1. temperaturepreviously heated to 85° C.
2. washThe TMEDA stripped product mixture was washed (3×300 ml) with deoxygenated water
3. customwere made at 80° C.
4. customWater and any rag or emulsion was removed through the bottom drain valve
5. temperatureThe temperature of the oil jacket was increased to 170° C
6. distillationResidual moisture and toluene were distilled through a simple distillation head (1 atm.)
7. customreached 161° C.
8. temperaturethe material was cooled
9. custompurged bottle (2918 g)

ORD record

ord-beb9ef1915154b9e956bfdae8e5d440a

Source dataset

uspto-grants-2015_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08933159B2