Acetic Acid → 1-Hexanol, 6-chloro-, 1-acetate

Temperature

10 °C

6-chlorohexanol (800 g) was added to anhydrous acetic acid (1,200 mL) cooled to 10° C. in an ice bath, and then pyridine (934 g) was dropped for 10 minutes. After the completion of dropping, they were refluxed for 2 hours. The reaction mixture was poured into water and toluene was further added and stirred. After neutralization the toluene layer with an aqueous saturated solution of sodium carbonate, it was washed with a small amount of water and further dried over anhydrous magnesium sulfate. Toluene and unreacted ingredients were distilled off from the toluene layer to obtain concentrates. The concentrates were purified by distillation under a reduced pressure to obtain 6-acetoxy chlorohexane (983 g). The boiling point was 82° C./5.3 hPa.

1. temperaturethey were refluxed for 2 hours
2. additionwas further added
3. washAfter neutralization the toluene layer with an aqueous saturated solution of sodium carbonate, it was washed with a small amount of water
4. dry with materialfurther dried over anhydrous magnesium sulfate
5. distillationToluene and unreacted ingredients were distilled off from the toluene layer
6. customto obtain concentrates
7. distillationThe concentrates were purified by distillation under a reduced pressure

ORD record

ord-f9244171a8b7484b9ca410d55842088e

Source dataset

uspto-grants-2008_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07393569B2