반응 #214211

반응 방정식

1,1,1-Tribromo-4-methyl-3-penten-2-ol

diketene

→

3-methyl-1-tribromomethyl-2-butenyl acetoacetate

수율 99.1%

용매

ether

반응 조건

후처리

1. 1
   기타were melted together at 90°
2. 2
   기타was then reduced to 80°
3. 3
   온도The resulting mixture was heated at 80° for three additional hours
4. 4
   온도After cooling
5. 5
   세척the ethereal solution was washed with 1 N aqueous hydrochloric acid
6. 6
   workup.ADDITIONThe washed mixture was treated with activated charcoal
7. 7
   건조dried over magnesium sulfate
8. 8
   기타Evaporation of the ether

실험 절차

1,1,1-Tribromo-4-methyl-3-penten-2-ol (6.72 g, 0.02 mole) and anhydrous sodium acetate (0.008 g) were melted together at 90°. The temperature of the mixture was then reduced to 80°, and diketene (about 2.6 ml, 0.022 mole) was added dropwise over a 10 minute period. The resulting mixture was heated at 80° for three additional hours. After cooling, the mixture was diluted with ether, and the ethereal solution was washed with 1 N aqueous hydrochloric acid and then ten times with saturated aqueous sodium bicarbonate. The washed mixture was treated with activated charcoal and dried over magnesium sulfate. Evaporation of the ether afforded 3-methyl-1-tribromomethyl-2-butenyl acetoacetate (8.34 g, 99% yield) as an oily residue.

출처