Nitrobenzene → 3-Nitrobenzenesulfonyl chloride

Temperature

82.5 °C

Chlorosulfonic acid (475 g) was taken in a 1 L three neck round bottom flask equipped with a guard tube and liquid addition funnel. Chlorosulfonic acid was cooled in an ice bath to 5-10° C. and nitrobenzene was added to the acid slowly, at such a rate that the temperature is maintained below 10° C. Reaction mixture was then brought to 25° C. and then slowly heated in an oil bath to 80-85° C. Reaction mixture was stirred further at 80-85° C. for 3 hours. After the completion of reaction (TLC), the reaction mixture was cooled to 10° C. and poured onto the ice-water mixture along with stirring and maintaining the temperature below 10° C.; the resulting slurry is then filtered on buchner funnel. Solid cake on funnel is washed with 500 mL of water. Resulting solid cake is dried on phosphorous pentoxide in a desiccator to obtain the D1 as off white solid.

1. customequipped with a guard tube and liquid addition funnel
2. temperatureat such a rate that the temperature is maintained below 10° C
3. customReaction mixture
4. customwas then brought to 25° C.
5. customReaction mixture
6. customAfter the completion of reaction (TLC)
7. temperaturethe reaction mixture was cooled to 10° C.
8. stirringwith stirring
9. temperaturemaintaining the temperature below 10° C.
10. filtrationthe resulting slurry is then filtered on buchner funnel
11. washSolid cake on funnel is washed with 500 mL of water
12. customResulting solid cake
13. customis dried on phosphorous pentoxide in a desiccator

ORD record

ord-1138bf747d1b4a2aaa4eccb0df5d06bd

Source dataset

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07998981B2