Nitrogen → 2-Iodo-1h,1h,2h,3h,3h-perfluoroalkan-1-ol (linear)

Temperature

60 °C

Into a 3-liter autoclave were poured 174 g (3.0 mol) of allyl alcohol, 49.2 g (0.3 mol) of α,α′-azobis isobutyronitrile (AIBN) and 300 ml of ethyl acetate. After decreasing the inside pressure (100 mmHg) on ice bath, N2 was introduced, and the inside pressure was decreased again. Thereafter, 588 g (3.0 mol) of CF3I was introduced and the mixture was slowly heated up to 60° C. After completion of the reaction, the reaction solution was cooled and washed with 1 mol/liter of an aqueous solution of HCl for separation of the solution. After that, refining by distillation was carried out, and 533 g (2.1 mol) of a fluorine-containing iodide (a): CF3CH2CHICH2OH was obtained.

1. customAfter completion of the reaction
2. temperaturethe reaction solution was cooled
3. washwashed with 1 mol/liter of an aqueous solution of HCl for separation of the solution
4. distillationAfter that, refining by distillation

ORD record

ord-7c7099b134c74f8f8dec90527b2bbf6a

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08871384B2