Reaktion #502088

Reaktionsgleichung

chloromethylether

Acetoxyethyloxymethylchloride

Triisopropylphosphite

→

Diisopropyl Phosphonate

Ausbeute 47.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONCollect 2-chloropropane distillate via short-path head in a dry ice cooled receiver, argon blanket, collected 140 g distillate (theoretical 157 g)
2. 2
   Sonstigereaction to yellow,
3. 3
   Temperaturcontinue heating another 2 h at 125° C. oil bath
4. 4
   workup.DISTILLATIONarrange for vacuum distillation
5. 5
   workup.DISTILLATIONDistilled a yellow front cut (140 g, head to 135° C., bottom to 190° C.)
6. 6
   SonstigeMain fraction was collected at head temperature of 178-187° C. (mostly 185-187° C.) with vacuum unknown at bath temperature of 222-228° C

Vorschrift

A 500 mL three-neck flask was charged with the crude chloromethylether 1 (317 g, 2.00 mol). Triisopropylphosphite (494 mL) was added dropwise through an additional funnel while heating in a 125° C. oil bath and stirring vigorously. Collect 2-chloropropane distillate via short-path head in a dry ice cooled receiver, argon blanket, collected 140 g distillate (theoretical 157 g). Phosphite blanched reaction to yellow, continue heating another 2 h at 125° C. oil bath, then arrange for vacuum distillation using a vacuum pump. Distilled a yellow front cut (140 g, head to 135° C., bottom to 190° C.), then changed to clean receiver. Main fraction was collected at head temperature of 178-187° C. (mostly 185-187° C.) with vacuum unknown at bath temperature of 222-228° C. 258 g of the product 2 was given (47% yield from 1,3-dioxolane).

Quelle