Hydrochloric Acid → HCID 87610807, compound

13 g (76 mmol) of 6,8-dimethylnon-7-enol (2), 10.8 g (107 mmol) of triethylamine and 200 ml of t-butyl methyl ether (MTBE) are placed in a 500 ml round-bottomed flask equipped with a thermometer and with a dropping funnel. Cooling is carried out to 5° C. and 8.4 g (107 mmol) of acetylchloride diluted in 20 ml of MTBE are added without exceeding a bulk temperature of 10° C. The mixture is stirred at ambient temperature for 14 hours. Cooling is carried out at 5° C. and neutralization is carried out with 100 ml of a 10% hydrochloric acid solution. The phases are separated and the organic phase is washed once with 100 ml of saturated aqueous NaHCO3 solution and then with aqueous saline solution to neutrality. The organic phase is dried and filtered, and the solvent is evaporated under reduced pressure. The acetate is purified by a distillation under reduced pressure (B.p.: 58° C./0.4 torr). The yield is 76%.

1. customequipped with a thermometer and with a dropping funnel
2. temperatureCooling
3. customis carried out to 5° C.
4. additionare added
5. customa bulk temperature of 10° C
6. temperatureCooling
7. customis carried out at 5° C.
8. customThe phases are separated
9. washthe organic phase is washed once with 100 ml of saturated aqueous NaHCO3 solution
10. customThe organic phase is dried
11. filtrationfiltered
12. customthe solvent is evaporated under reduced pressure
13. distillationThe acetate is purified by a distillation under reduced pressure (B.p.: 58° C./0.4 torr)

ORD record

ord-8a0cfead0535481bb11cf20b7fe8c21b

Source dataset

uspto-grants-2009_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07501536B2