Reacción #703228

Ecuación de reacción

αmethylol benzoin

paraldehyde

→

yellow oil

Rendimiento 107.3%

2-methyl-4-phenyl-4-benzoyl-1,3-dioxolane

Rendimiento 107.3%

Disolventes

benzene

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturathat refluxing
2. 2
   Otrothe vapors condensed
3. 3
   TemperaturaThe temperature of the reaction mixture was then gradually raised to 120°-130° C
4. 4
   Otrowater was collected
5. 5
   Otrosaturated with ammonia gas, the resulting salt precipitate removed by filtration on a Buchner funnel
6. 6
   Otroto provide a benzene solution of the reaction product
7. 7
   OtroThe benzene solvent was removed under vacuum

Procedimiento

A solution of 10.0 grams (41 millimoles)αmethylol benzoin, 20.0 grams (45 millimoles) paraldehyde, 0.5 grams p-toluenesulfonic acid and 100 ml. benzene was heated with magnetic stirring to 80°-90° C for 30 minutes under a Dean-Stark trap under conditions such that refluxing occurred, but the vapors condensed before reaching the trap. The temperature of the reaction mixture was then gradually raised to 120°-130° C and 8 ml. water was collected. The reaction mixture was then saturated with ammonia gas, the resulting salt precipitate removed by filtration on a Buchner funnel to provide a benzene solution of the reaction product. The benzene solvent was removed under vacuum. A yield of 11.8 grams of a yellow oil was obtained. The yellow oil was chromatographed on silica gel with 5% ethyl ether in n-hexane elution to provide 9.5 grams of an odorous yellow oil which distilled at 125°-130° C at 20μ vacuum pressure to provide 6.5 grams of a light yellow oil product.

Fuente