Reaktion #214358

Reaktionsgleichung

isobutylene

2,4,4,4-tetrachlorobutyryl chloride

triethylamine

→

2-chloro-2-(2',2',2'-trichloroethyl)-3,3-dimethylcyclobutan-1-one

Ausbeute 60.2%

Lösungsmittel

cyclohexane

cyclohexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis then pumped in at 65° C
2. 2
   FiltrationThe precipitated hydrochloride of triethylamine is collected by filtration
3. 3
   Einengenthe filtrate is concentrated
4. 4
   FiltrationThe resulting crystals are collected by filtration

Vorschrift

In an autoclave, 280 g of isobutylene are added under pressure to 122 g (0.5 mole) of 2,4,4,4-tetrachlorobutyryl chloride in 600 ml of cyclohexane. A solution of 51 g (0.5 mole) of triethylamine in 500 ml of cyclohexane is then pumped in at 65° C. The reaction mixture is then kept for 3 hours at 65° C. The precipitated hydrochloride of triethylamine is collected by filtration and the filtrate is concentrated. The resulting crystals are collected by filtration, affording 79.4 g of 2-chloro-2-(2',2',2'-trichloroethyl)-3,3-dimethylcyclobutan-1-one with a melting point of 75°-76° C. (60% of theory).

Quelle