반응 #684163

반응 방정식

sodium bicarbonate

trioxane

isobutyric anhydride

perchloric acid

→

methylene bisisobutyrate

반응 조건

후처리

1. 1
   기타decreased to 27° C
2. 2
   추출extracted with ether
3. 3
   건조The ether extracts were dried over magnesium sulfate
4. 4
   기타evaporated under reduced pressure
5. 5
   workup.DISTILLATIONThe resulting residue was distilled on a 30-cm column

실험 절차

A 30-g (0.33 mol) sample of trioxane was added to a solution of 158 g (1 mol) isobutyric anhydride and 0.5 ml 70% perchloric acid over a 30-minute period at 65°-70° C. The reaction mixture was then stirred until the temperature decreased to 27° C. The reaction mixture was diluted with saturated sodium bicarbonate solution and extracted with ether. The ether extracts were dried over magnesium sulfate and evaporated under reduced pressure. The resulting residue was distilled on a 30-cm column to give 112 g of methylene bisisobutyrate, b.p. 43°-48° C. at 0.2-0.3 mm of Hg and 30 g of oxybis-methylene isobutyrate, b.p. 57°-63° C. at 0.2-0.3 mm of Hg.

출처