Acetic Acid → HCID 13092422, compound

82 g (1.2 mol) of Isoprene and 360 g of glacial acetic acid were mixed. With stirring under ice cooling and with keeping an internal temperature at 10°-15° C., 108 g (1.0 mol) of t-butyl hypochlorite were added dropwise therein. The resulting mixture was continuously stirred as it was until the yellow color of said t-butyl hypochlorite disapperared from the reaction liquid. After water (500 ml) was added into the reaction liquid, it was extracted with ether (300 ml×2). After the organic layer was washed with an aqueous solution saturated with sodium hydrogencarbonate, and thereafter with water and dried, it was concentrated under reduced pressure, thereby obtaining an oily residue. This residue was distilled under reduced pressure, whereby 120 g of the title compound were obtained. (Yield: 43%)

1. customat 10°-15° C.
2. stirringThe resulting mixture was continuously stirred as it
3. customdisapperared from the reaction liquid
4. extractionwas extracted with ether (300 ml×2)
5. washAfter the organic layer was washed with an aqueous solution saturated with sodium hydrogencarbonate
6. dry with materialwith water and dried
7. concentrationit was concentrated under reduced pressure
8. customobtaining an oily residue
9. distillationThis residue was distilled under reduced pressure

ORD record

ord-2698200f961b4654859094bd90fd540f

Source dataset

uspto-grants-1996_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05565586