反应详情

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.

1. customdecreased to 27° C
2. extractionextracted with ether
3. dry with materialThe ether extracts were dried over magnesium sulfate
4. customevaporated under reduced pressure
5. distillationThe resulting residue was distilled on a 30-cm column